Establishment and maintenance of low gas pressure within interior spaces of temperature-stabilized storage systems

ABSTRACT

Methods and apparatus described herein relate to establishing and maintaining low gas pressure within a gas-sealed device fabricated from heat sensitive materials. Methods include transferring activated getters within the interior of an apparatus from regions fabricated from heat-resistant materials to interior regions of the gas-sealed device fabricated from heat-sensitive materials.

CROSS-REFERENCE TO RELATED APPLICATIONS

The present application is related to and claims the benefit of theearliest available effective filing date(s) from the following listedapplication(s) (the “Related applications”) (e.g., claims earliestavailable priority dates for other than provisional patent applicationsor claims benefits under 35 USC §119(e) for provisional patentapplications, for any and all parent, grandparent, great-grandparent,etc. applications of the Related application(s)). All subject matter ofthe Related applications and of any and all parent, grandparent,great-grandparent, etc. applications of the Related applications,including any priority claims, is incorporated herein by reference tothe extent such subject matter is not inconsistent herewith.

RELATED APPLICATIONS

-   -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/001,757, entitled        TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming Roderick A.        Hyde; Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T.        Tegreene; William H. Gates, III; Charles Whitmer; and Lowell L.        Wood, Jr. as inventors, filed Dec. 11, 2007, which is currently        co-pending, or is an application of which a currently co-pending        application is entitled to the benefit of the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/006,088, entitled        TEMPERATURE-STABILIZED STORAGE CONTAINERS WITH DIRECTED ACCESS,        naming Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold;        Clarence T. Tegreene; William H. Gates, III; Charles Whitmer;        and Lowell L. Wood, Jr. as inventors, filed Dec. 27, 2007, which        is currently co-pending, or is an application of which a        currently co-pending application is entitled to the benefit of        the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/006,089, entitled        TEMPERATURE-STABILIZED STORAGE SYSTEMS, naming Roderick A. Hyde;        Edward K. Y. Jung; Nathan P. Myhrvold; Clarence T. Tegreene;        William H. Gates, III; Charles Whitmer; and Lowell L. Wood, Jr.        as inventors, filed Dec. 27, 2007, which is currently        co-pending, or is an application of which a currently co-pending        application is entitled to the benefit of the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/008,695, entitled        TEMPERATURE-STABILIZED STORAGE CONTAINERS FOR MEDICINALS, naming        Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold;        Clarence T. Tegreene; William H. Gates, III; Charles Whitmer;        and Lowell L. Wood, Jr. as inventors, filed Jan. 10, 2008, which        is currently co-pending, or is an application of which a        currently co-pending application is entitled to the benefit of        the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/012,490, entitled METHODS OF        MANUFACTURING TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming        Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold;        Clarence T. Tegreene; William H. Gates, III; Charles Whitmer;        and Lowell L. Wood, Jr. as inventors, filed Jan. 31, 2008, which        is currently co-pending, or is an application of which a        currently co-pending application is entitled to the benefit of        the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/077,322, entitled        TEMPERATURE-STABILIZED MEDICINAL STORAGE SYSTEMS, naming        Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold;        Clarence T. Tegreene; William Gates; Charles Whitmer; and        Lowell L. Wood, Jr. as inventors, filed Mar. 17, 2008, which is        currently co-pending, or is an application of which a currently        co-pending application is entitled to the benefit of the filing        date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/152,465, entitled STORAGE        CONTAINER INCLUDING MULTI-LAYER INSULATION COMPOSITE MATERIAL        HAVING BANDGAP MATERIAL AND RELATED METHODS, naming Jeffrey A.        Bowers; Roderick A. Hyde; Muriel Y. Ishikawa; Edward K. Y. Jung;        Jordin T. Kare; Eric C. Leuthardt; Nathan P. Myhrvold; Thomas J.        Nugent Jr.; Clarence T. Tegreene; Charles Whitmer; and Lowell L.        Wood Jr. as inventors, filed May 13, 2008, which is currently        co-pending, or is an application of which a currently co-pending        application is entitled to the benefit of the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/152,467, entitled MULTI-LAYER        INSULATION COMPOSITE MATERIAL INCLUDING BANDGAP MATERIAL,        STORAGE CONTAINER USING SAME, AND RELATED METHODS, naming        Jeffrey A. Bowers; Roderick A. Hyde; Muriel Y. Ishikawa;        Edward K. Y. Jung; Jordin T. Kare; Eric C. Leuthardt; Nathan P.        Myhrvold; Thomas J. Nugent Jr.; Clarence T. Tegreene; Charles        Whitmer; and Lowell L. Wood Jr. as inventors, filed May 13,        2008, which is currently co-pending, or is an application of        which a currently co-pending application is entitled to the        benefit of the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/220,439, entitled MULTI-LAYER        INSULATION COMPOSITE MATERIAL HAVING AT LEAST ONE        THERMALLY-REFLECTIVE LAYER WITH THROUGH OPENINGS, STORAGE        CONTAINER USING SAME, AND RELATED METHODS, naming Roderick A.        Hyde; Muriel Y. Ishikawa; Jordin T. Kare; and Lowell L. Wood,        Jr. as inventors, filed Jul. 23, 2008, which is currently        co-pending, or is an application of which a currently co-pending        application is entitled to the benefit of the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/658,579, entitled        TEMPERATURE-STABILIZED STORAGE SYSTEMS, naming Geoffrey F.        Deane; Lawrence Morgan Fowler; William Gates; Zihong Guo;        Roderick A. Hyde; Edward K. Y. Jung; Jordin T. Kare; Nathan P.        Myhrvold; Nathan Pegram; Nels R. Peterson; Clarence T. Tegreene;        Charles Whitmer; and Lowell L. Wood, Jr. as inventors, filed        Feb. 8, 2010, which is currently co-pending, or is an        application of which a currently co-pending application is        entitled to the benefit of the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/927,981, entitled        TEMPERATURE-STABILIZED STORAGE SYSTEMS WITH FLEXIBLE CONNECTORS,        naming Fong-Li Chou; Geoffrey F. Deane; William Gates; Zihong        Guo; Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold;        Nels R. Peterson; Clarence T. Tegreene; Charles Whitmer; and        Lowell L. Wood, Jr. as inventors, filed Nov. 29, 2010, which is        currently co-pending, or is an application of which a currently        co-pending application is entitled to the benefit of the filing        date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 12/927,982, entitled        TEMPERATURE-STABILIZED STORAGE SYSTEMS INCLUDING STORAGE        STRUCTURES CONFIGURED FOR INTERCHANGEABLE STORAGE OF MODULAR        UNITS, naming Geoffrey F. Deane; Lawrence Morgan Fowler; William        Gates; Jenny Ezu Hu; Roderick A. Hyde; Edward K. Y. Jung;        Jordin T. Kare; Nathan P. Myhrvold; Nathan Pegram; Nels R.        Peterson; Clarence T. Tegreene; Charles Whitmer; and Lowell L.        Wood, Jr. as inventors, filed Nov. 29, 2010, which is currently        co-pending, or is an application of which a currently co-pending        application is entitled to the benefit of the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 13/135,126, entitled        TEMPERATURE-STABILIZED STORAGE SYSTEMS CONFIGURED FOR STORAGE        AND STABILIZATION OF MODULAR UNITS, naming Geoffrey F. Deane;        Lawrence Morgan Fowler; William Gates; Jenny Ezu Hu; Roderick A.        Hyde; Edward K. Y. Jung; Jordin T. Kare; Mark K. Kuiper;        Nathan P. Myhrvold; Nathan Pegram; Nels R. Peterson; Clarence T.        Tegreene; Mike Vilhauer; Charles Whitmer; Lowell L. Wood, Jr.;        and Ozgur Emek Yildirim as inventors, filed Jun. 23, 2011, which        is currently co-pending, or is an application of which a        currently co-pending application is entitled to the benefit of        the filing date.    -   For purposes of the USPTO extra-statutory requirements, the        present application constitutes a continuation-in-part of U.S.        patent application Ser. No. 13/199,439, entitled METHODS OF        MANUFACTURING TEMPERATURE-STABILIZED STORAGE CONTAINERS, naming        Roderick A. Hyde; Edward K. Y. Jung; Nathan P. Myhrvold;        Clarence T. Tegreene; William H. Gates, III; Charles Whitmer;        and Lowell L. Wood, Jr. as inventors, filed Aug. 29, 2011, which        is currently co-pending, or is an application of which a        currently co-pending application is entitled to the benefit of        the filing date.

The United States Patent Office (USPTO) has published a notice to theeffect that the USPTO's computer programs require that patent applicantsreference both a serial number and indicate whether an application is acontinuation, continuation-in-part, or divisional of a parentapplication. Stephen G. Kunin, Benefit of Prior-Filed Application, USPTOOfficial Gazette Mar. 18, 2003. The present Applicant Entity(hereinafter “Applicant”) has provided above a specific reference to theapplication(s) from which priority is being claimed as recited bystatute. Applicant understands that the statute is unambiguous in itsspecific reference language and does not require either a serial numberor any characterization, such as “continuation” or“continuation-in-part,” for claiming priority to U.S. patentapplications. Notwithstanding the foregoing, Applicant understands thatthe USPTO's computer programs have certain data entry requirements, andhence Applicant has provided designation(s) of a relationship betweenthe present application and its parent application(s) as set forthabove, but expressly points out that such designation(s) are not to beconstrued in any way as any type of commentary and/or admission as towhether or not the present application contains any new matter inaddition to the matter of its parent application(s).

SUMMARY

Apparatus described herein include, but are not limited to: a structuralregion fabricated from a heat-sensitive material, the structural regionincluding an outer wall and an inner wall with a gas-sealed gap betweenthe outer wall and the inner wall; an activation region fabricated froma heat-resistant material, the activation region including one or moregetters; a connector attached to the structural region and to theactivation region, the connector including a flexible region and aregion configured for sealing and detachment of the structural regionfrom the activation region; and a vacuum pump operably attached to theconnector.

Methods described herein include, but are not limited to: establishingvacuum within a gas-sealed apparatus including at least one activationregion fabricated from a heat-resistant material, a structural regionfabricated from a heat-sensitive material, and a connector between theregions; heating the at least one activation region to an activationtemperature for an activation time suitable to activate one or moregetters within the at least one activation region, while maintaining theestablished vacuum within the gas-sealed apparatus; allowing the atleast one activation region and the one or more getters to cool to atemperature compatible with structural stability of the heat-sensitivematerial; transferring the cooled one or more getters from the cooled atleast one activation region to the structural region through theconnector, while maintaining the established vacuum within theapparatus; and separating the connector between the regions whilemaintaining the vacuum within the structural region including the cooledone or more getters. Methods of establishing and maintaining vacuumwithin a storage device also include, but are not limited to: assemblingsubstantially all structural components of a storage device, includingan outer wall and an inner wall substantially defining a gas-sealed gap;attaching the storage device to a gas-sealed apparatus, the gas-sealedapparatus including a getter activation region containing one or moregetters, a vacuum pump, and a connector operably connecting the storagedevice to the gas-sealed apparatus; activating the vacuum pump toestablish gas pressure below atmospheric pressure within the gas-sealedgap of the storage device; heating the storage device to a predeterminedtemperature for a predetermined length of time; heating the getteractivation region and the one or more getters to an activationtemperature for an activation time suitable to activate one or moregetters within the at least one getter activation region, whilemaintaining the established gas pressure below atmospheric pressurewithin the gas-sealed gap of the storage device; allowing the getteractivation region and the one or more getters to cool to a predeterminedtemperature; flexing the connector to move the storage device and thegetter activation region into a relative position wherein the getteractivation region is above the storage device and the connector issubstantially linear; allowing the getters to fall along the connectorinterior into the gas-sealed gap in the storage device, whilemaintaining the established gas pressure below atmospheric pressurewithin the gas-sealed gap of the storage device; separating theconnector at a location adjacent to the storage device while maintainingthe established gas pressure below atmospheric pressure within thegas-sealed gap of the storage device. In addition to the foregoing,other method aspects are described in the claims, drawings, and textforming a part of the present disclosure.

In addition to the foregoing, other aspects are described in the claims,drawings, and text forming a part of the present disclosure. Theforegoing summary is illustrative only and is not intended to be in anyway limiting. In addition to the illustrative aspects, embodiments, andfeatures described above, further aspects, embodiments, and featureswill become apparent by reference to the drawings and the followingdetailed description.

BRIEF DESCRIPTION OF THE FIGURES

FIG. 1 is a schematic of an apparatus.

FIG. 2 is a schematic of an apparatus such as that illustrated in FIG.1.

FIG. 3 is a schematic of an apparatus such as that depicted in FIGS. 1and 2.

FIG. 4 is a schematic of an apparatus such as that depicted in FIGS. 1,2 and 3.

FIG. 5 depicts a flowchart of a method.

FIG. 6 illustrates a flowchart of a method.

FIG. 7 shows a flowchart of a method such as illustrated in FIG. 6.

FIG. 8 depicts a flowchart of a method such as illustrated in FIG. 6.

FIG. 9 illustrates a flowchart of a method such as illustrated in FIG.6.

FIG. 10 shows a flowchart of a method such as illustrated in FIG. 6.

FIG. 11 depicts a flowchart of a method such as illustrated in FIG. 6.

FIG. 12 illustrates a flowchart of a method such as illustrated in FIG.6.

FIG. 13 shows a flowchart of a method such as illustrated in FIG. 6.

FIG. 14 depicts a flowchart of a method such as illustrated in FIG. 6.

FIG. 15 illustrates a flowchart of a method such as illustrated in FIG.6.

FIG. 16 illustrates a flowchart of a method.

FIG. 17 shows a flowchart of a method such as illustrated in FIG. 16.

FIG. 18 depicts a flowchart of a method such as illustrated in FIG. 16.

FIG. 19 illustrates a flowchart of a method such as illustrated in FIG.16.

FIG. 20 shows a flowchart of a method such as illustrated in FIG. 16.

FIG. 21 depicts a flowchart of a method such as illustrated in FIG. 16.

FIG. 22 illustrates a flowchart of a method such as illustrated in FIG.16.

FIG. 23 is a schematic of a storage container.

DETAILED DESCRIPTION

In the following detailed description, reference is made to theaccompanying drawings, which form a part hereof. In the drawings,similar symbols typically identify similar components, unless contextdictates otherwise. The illustrative embodiments described in thedetailed description, drawings, and claims are not meant to be limiting.Other embodiments may be utilized, and other changes may be made,without departing from the spirit or scope of the subject matterpresented here.

The use of the same symbols in different drawings typically indicatessimilar or identical items.

Methods and apparatus described herein are useful to establish andmaintain a stable and extremely low gas pressure within an internal,gas-sealed region of a container. Methods and apparatus as describedherein have a variety of potential uses in the manufacture of containersthat include internal, gas-sealed regions with durable gas pressurebelow atmospheric pressure, such as near-vacuum gas pressure, withoutactive pumping of gas out of the internal gas-sealed regions. Methodsand apparatus described herein may be utilized to establish and maintaina durable low gas pressure region internal to a container structure, andmay be particularly useful in regard to containers fabricated frommaterials that lose their structural stability at temperatures below theactivation temperatures required by many getter materials. For example,the methods and apparatus as described herein may be utilized toestablish and maintain a stable gas pressure below atmospheric pressure,such as near-vacuum gas pressure, within an internal, gas-sealed cavitywithin a portion of a larger device fabricated all or in part fromaluminum. For example, the methods and apparatus as described herein maybe useful in the manufacture and durability of containers fabricated outof plastic-metal composites that include internal, gas-impermeablespaces with gas pressure less than that of the environment surroundingthe container, such as substantially evacuated, gas-impermeable internalspaces.

Internal, gas-sealed regions with low gas pressure may be incorporatedinto the structure of containers as part of the insulation for thecontainer. Internal, gas-sealed regions of low gas pressure incorporatedinto the structure of containers as partial insulation for the containermay include other materials or features, such as insulation materials,electronics or structural features of the container. For example,internal, gas-sealed regions of low gas pressure incorporated into thestructure of a container may include multilayer insulation material(MLI). For example, internal, gas-sealed regions of low gas pressureincorporated into the structure of a container may include wires orconduits connecting electronic components operably attached to differentregions of the container. Internal, gas-sealed regions of low gaspressure may also isolate electronics incorporated into the device fromexternal factors, such as chemically active materials, magneticallyactive materials, water, heat and cold. For example, internal,gas-sealed regions of low gas pressure incorporated into the structureof a container may include structural elements such as flanges,supports, struts and other features improving the structural stabilityof the container. Internal, gas-sealed regions of low pressure may haveadvantages of low weight and cost in a finished, manufactured device.Methods and apparatus described herein may be used to manufacturesubstantially thermally sealed storage devices, such as those suitablefor stable maintenance of stored materials within a predeterminedtemperature range without reliance on external power sources to maintainthe temperature range within the storage area. For example, containersand devices such as those manufactured with the methods and apparatusdescribed herein are suitable for maintenance of stored materials withina predetermined temperature range in locations with minimal municipalpower, or unreliable municipal power sources, such as remote locationsor in emergency situations. For example, containers and devices such asthose manufactured with the methods and apparatus described herein maybe useful for the transport and storage of materials that are sensitiveto external temperature changes that can occur during shipment andstorage. For example, the storage systems described herein are usefulfor the shipment and storage of medicinal agents, including vaccines.

Many medicinal agents, including vaccines, currently in regular use arehighly sensitive to temperature variations, and must be maintained in aparticular temperature range to preserve stability, as well as thepotency and efficacy of the medicinal agents. The temperature range tomaintain stability in storage is inherent to the particular formulationand medicinal agent. For example, many medicinal agents, includingvaccines, must be stored in a predetermined temperature range, such asbetween 2 degrees Centigrade and 8 degrees Centigrade, or between 0degrees Centigrade and 10 degrees Centigrade, or between 10 degreesCentigrade and 15 degrees Centigrade, or between 15 degrees Centigradeand 25 degrees Centigrade, or between −15 degrees Centigrade and −5degrees Centigrade, or between −50 degrees Centigrade and −15 degreesCentigrade, to preserve efficacy of the medicinal agent. Storage andtransport of medicinal agents, including vaccines, within a temperaturerange, such as between 2 degrees Centigrade and 8 degrees Centigrade, orbetween 0 degrees Centigrade and 10 degrees Centigrade, or between 10degrees Centigrade and 15 degrees Centigrade, or between 15 degreesCentigrade and 25 degrees Centigrade, or between −15 degrees Centigradeand −5 degrees Centigrade, or between −50 degrees Centigrade and −15degrees Centigrade, is often referred to as the “cold chain.”

Health care providers and clinics who use medicinal agents, such asvaccines, must follow established protocols and procedures formaintenance of the cold chain, including during transport and in timesof emergency and in power failures, to ensure medicinal agent activitysuch as vaccine potency. See: Rodgers et al., “Vaccine Cold Chain Part 1Proper Handling and Storage of Vaccine,” AAOHN Journal 58(8) 337-344(2010); Rodgers et al., “Vaccine Cold Chain Part 2: Training Personneland Program Management,” AAOHN Journal 8(9): 391-402 (2010); Magennis etal., “Pharmaceutical Cold Chain” A Gap in the Last Mile,” Pharmaceutical& Medical Packaging News, 44-50 (September 2010); and Kendal et al.,“Validation of Cold Chain Procedures Suitable for Distribution ofVaccines by Public Health Programs in the USA,” Vaccine 15 (12/13):1459-1465 (1997) which are each incorporated by reference. For example,failure to follow established protocols and procedures for maintenanceof the cold chain, even during periods of normal use in developedcountries, leads to significant levels of vaccine wastage due toexposure to both excessively high and excessively low temperatures. Insome cases, a brief period outside of normal storage temperatures issufficient to disrupt activity. See: Thakker and Woods, “Storage ofVaccines in the Community: Weak Link in the Cold Chain?” British MedicalJournal 304: 756-758 (1992); Matthias et al., “Freezing Temperatures inthe Vaccine Cold Chain: A Systematic Literature Review,” Vaccine 25:3980-3986 (2007); Edsam et al., “Exposure of Hepatitis B Vaccine toFreezing Temperatures During Transport to Rural Health Centers inMongolia,” Preventative Medicine 39: 384-388 (2004); Techathawat et al.,“Exposure to Heat and Freezing in the Vaccine Cold Chain in Thailand,”Vaccine 25: 1328-1333 (2007); and Setia et al., “Frequency and Causes ofVaccine Wastage,” Vaccine 20: 1148-1156 (2002), which are eachincorporated by reference. Although some breaks in cold chainmaintenance, such as frozen vaccine vials and vials containingprecipitants due to improper temperature exposure, may be readilyapparent, medicinal agents such as vaccines with reduced potency due tobreaks in cold chain maintenance may not be readily detectable. See:Chen et al., “Characterization of the Freeze Sensitivity of a HepatitisB Vaccine,” Human Vaccines 5(1): 26-32 (2009), which is incorporated byreference. Medicinal agent stocks with reduced potency or efficacy dueto exposure to excessively high temperatures may not be immediatelyidentifiable. The temperature sensitivity of any given medicinal agentvaries widely depending on the specific agent, or example the specificvaccine formulation. In some circumstances, a few minutes outside of theappropriate temperature range can significantly impact the biologicaleffectiveness of a particular container of a medicinal agent. See:Kristensen and Chen, “Stabilization of Vaccines: Lessons Learned,” HumanVaccines 6(3): 229-230 (2010), which is incorporated by reference.Issues related to the maintenance of cold chain are even moresignificant in less well developed regions of the world. See: Wirkas etal., “A Vaccine Cold Chain Freezing Study in PNG Highlights TechnologyNeeds for Hot Climate Countries,” Vaccine 25: 691-697 (2007); and Nelsonet al., “Hepatitis B Vaccine Freezing in the Indonesian Cold Chain:Evidence and Solutions,” Bulletin of the World Health Organization,82(2): 99-105 (2004), which are each incorporated by reference. Inaddition, approaches to the cold chain that require less energy may bedesirable for ongoing cost and climate considerations. See Halldórssonand Kovacs, “The Sustainable Agenda and Energy Efficiency: LogisticsSolutions and Supply Chains in Times of Climate Change,” InternationalJournal of Physical Distribution & Logistics Management 40 (1/2): 5-13(2010), which is incorporated by reference. Thermal stabilization ofmedicinal agents, such as vaccines, for use beyond the cold chainincludes economic, logistical, regulatory, procurement and policy issues(see Kristensen and Chen, “Stabilization of vaccines: lessons learned,”Human Vaccines, vol. 6, no. 3, March 2010, pages 229-231, which isincorporated by reference).

Containers and storage devices such as those fabricated using methodsand apparatus described herein may be designed in a variety of sizes andshapes, depending on the embodiment. For example, containers and storagedevices may be fabricated in various sizes, shapes and materialsdepending on the intended use of the container or storage device. Arepresentative example of a storage container is shown in FIG. 23 anddescribed in the associated text (see below). For example, containersand storage devices manufactured using the methods and apparatusdescribed herein may be of a shape and size for convenient portability,such as no more than 1 kilogram (kg), 2 kg, 5 kg, 7 kg or 10 kg. Forexample, containers and storage devices manufactured using the methodsand apparatus described herein may be of a size and shape to be carriedeasily by an individual person, either directly or with a carrier, suchas with a satchel, duffle bag, rucksack, carryall, handbag, haversack,knapsack, pack, pouch, suitcase, tote, travel bag or backpack. Forexample, containers and storage devices may be fabricated in a shape andsize for transport using a small wheeled conveyance operated by a singleperson, such as with a mass of no more than 15 kg, 20 kg, or 25 kg. Forexample, containers and storage devices manufactured using the methodsand apparatus described herein may be of a size and shape to be carriedeasily by a person using a handcart, a rickshaw, a gurney, a bicycle ora motorcycle, such as in a saddlebag, carrier or rack. For example,containers and storage devices may be fabricated in a shape and size fortransport using a truck, wagon, pickup, van or other motorized deliveryvehicle, such as with a mass of no more than 30 kg, 35 kg, 40 kg, 45 kg,50 kg or 55 kg. For example, containers and storage devices may befabricated in a shape and size for substantially stationary use, forexample with a mass of greater than 100 kg.

Apparatus

With reference now to FIG. 1, shown is an example of an apparatus thatmay serve as a context for the subject matter described herein. FIG. 1illustrates a schematic of an apparatus 185. The apparatus 185 includesa structural region 180, an activation region 100, a connector 120attached to the structural region 180 and to the activation region 100,and a vacuum pump 130. Each of the structural region 180, the activationregion 100, the connector, and the vacuum pump 130 includes an internal,gas-sealed region. For example, the structural region 180 includes agas-sealed gap 145 between the outer wall 150 and the inner wall 155.The entire apparatus 185 includes an internal, gas-sealed region that iscontiguous throughout the regions (e.g. 100, 120, 145) of the apparatus185.

The structural region 180 is fabricated from a heat-sensitive material.The structural region 180 may be fabricated entirely or in part from aheat-sensitive material. The structural region 180 may be fabricatedfrom a combination of materials. Wherein the structural region includescomponents fabricated from different materials, the material with thelowest heat tolerance will govern the heat-sensitivity of the entirestructural region 180. The structural region 180 includes an outer wall150 and an inner wall 155, with a gas-sealed gap 145 between the outerwall 150 and the inner wall 155. The activation region 100 is fabricatedfrom a heat-resistant material. The activation region 100 is entirelyfabricated from a heat-resistant material utilizing methods that arealso heat-resistant. For example, any epoxy, seals, coatings or similarcomponents within the activation region 100 structure will beheat-resistant. Wherein the activation region includes componentsfabricated from different materials, the material with the lowest heattolerance will govern the heat-resistance of the entire activationregion 100. The activation region 100 includes one or more getters 110.

The connector 120 is attached to both the structural region 180 and theactivation region 100. The connector 120 is operably connected to boththe structural region 180 and the activation region 100 withgas-impermeable connections to form a gas-sealed interior. For example,the connector 120 may be attached to the structural region 180 and theactivation region 100 using gas-impermeable seals on the respective endsof the connector 120. For example, the connector 120 may be welded on tothe structural region 180 and the activation region 100 on therespective ends of the connector 120 to form a gas-impermeable weldingjoint. The connector 120 includes a flexible region 125. The connectorincludes a region 127 configured for sealing and detachment of thestructural region 180 from the activation region 100. The vacuum pump130 is operably attached to the connector 120. The vacuum pump 130 isoperably attached to the connector 120 to allow the vacuum pump 130 tosubstantially evacuate the gas within the gas-sealed interior of theapparatus 185 during utilization of the methods described herein. Insome embodiments, the vacuum pump 130 may be operably attached to theconnector 120 through a tube, duct, conduit or other structure thatcreates a gas-impermeable seal between the vacuum pump 130 and theconnector 120. FIG. 1, for example, illustrates the vacuum pump 130 asoperably attached to the connector 120 through a conduit 170.

The apparatus 185 includes a gas-sealed interior region throughout thestructural region 180, the activation region 100, and the connector 120attached to the structural region 180 and to the activation region 100.Gas-impermeable seals are located in each of the junctions betweenregions 180, 100 of the apparatus 185 and the connector. The vacuum pump130 is also operably attached to the connector 120 with agas-impermeable seal. See: Ishimaru, “Bakable aluminum vacuum chamberand bellows with an aluminum flange and metal seal for ultrahighvacuum,” Journal of Vacuum Science and Technology, vol. A15, no. 6,November/December 1978, pages 1853-1854; and Jhung et al., “Achievementof extremely high vacuum using a cryopump and conflate aluminumgaskets,” Vacuum, vol. 43, no. 4, 1992, pages 309-311; which are eachincorporated by reference. The vacuum pump 130 may be attached to theconnector 120 through a through a structure, such as conduit 170, thatincludes a gas-impermeable seal between the vacuum pump 130 and theconnector 120. The vacuum pump 130 included in a specific embodimentshould have sufficient pumping capacity to substantially evacuate theentirety of the gas-sealed interior region throughout the structuralregion 180, the activation region 100, and the connector 120 attached tothe structural region 180 and to the activation region 100.

A valve 135 may be operably attached to the connector 120, for examplein the region of the connector 120 between the attached vacuum pump 130and conduit 170 and the attached structural region 180. A valve 135operably attached to the connector 120 may be configured to inhibit theflow of gas through the connector 120. A valve 135 operably attached tothe connector 120 may be configured to block the flow of gas through theconnector 120. A valve 135 operably attached to the connector 120 isconfigured to restrict gas flow through the interior of the connector120 at a location along the length of the connector 120. For example, asillustrated in FIG. 1, a valve 135 may be configured to prevent gas flowbetween the gas-sealed gap 145 in the structural region 180 from theflexible region 125 of the connector 120, and the interior of theactivation region 100. As an example, as illustrated in FIG. 1, a valve135 may be integrated into the connector 120 and configured toreversibly prevent the flow of gas within the interior of the connector120. A valve 135 may be configured to isolate gas present in one regionof the interior of the apparatus 185 from another region of the interiorof the apparatus 185. A valve 135 may be of a number of types, asappropriate to the embodiment and relative to factors such as cost,size, durability, structural strength, outgassing of fabricationmaterials, and sealing strength. A valve 135 may be a quarter-turnvalve, such as a butterfly style valve. A valve 135 may be a ball valve.In some embodiments, there may be a plurality of valves. If a valve 135includes organic materials, such as nitrile, in “O” rings or othercomponents, the expected outgassing rate of the value components shouldbe understood to effect the time required to achieve a target minimalgas pressure within the apparatus. See: L. de Csernatony, “Theproperties of Viton “A” elastomers II: the influence of permeation,diffusion and solubility of gases on the gas emission rate from anO-ring used as an atmospheric seal or high vacuum immersed,” Vacuum,vol. 16, no. 3, 1965, pages 129-134, which is incorporated by reference.In some embodiments, baking the value under vacuum conditions prior toassembly of the apparatus (e.g. see FIG. 5 and associated text) mayreduce outgassing from organic materials within the valve. See: D. J.Crawley and L. de Csernatony, “Degassing characteristics of some ‘O’ring materials,” Vacuum, vol. 14, 1964, pages 7-9; and S. Rutherford,“The benefits of Viton outgassing,” Duniway Stockroom Corp., 1997, pages1-5, which are each incorporated by reference.

The structural region 180 fabricated from a heat-sensitive materialincludes a device configured for use independently from the remainder ofthe apparatus. For example, the structural region 180 may include astorage device (see, e.g. FIG. 23) configured for use independently fromthe remainder of the apparatus. For example, the structural region 180may include a storage device (see, e.g. FIG. 23) configured for useindependently from the connector 120, the vacuum pump 130 and theactivation region 100. For example, the structural region 180 mayinclude a substantially thermally sealed container configured for useindependently from the connector 120, the vacuum pump 130 and theactivation region 100. In some embodiments, the structural region 180includes a device configured for detachment from the remainder of theapparatus. In some embodiments, the structural region 180 includes astorage device. In some embodiments, the structural region 180 includesa storage device configured for temperature-stabilized storage. In someembodiments, the structural region 180 includes a thermally-insulateddevice. The structural region 180 may include a storage device with aninterior storage region 165 and an opening 160 in the structural region180 of a suitable size and shape to maintain the thermal storageproperties of the interior storage region 165 and to allow for theaddition and removal of any stored material within the interior storageregion 165. The interior storage region 165 is a substantially thermallysealed storage region containing an access opening 160 of minimal sizeand shape to allow insertion and removal of stored material from theinterior storage region 165. The storage device may include a container,such as a thermally-stabilized container (see, e.g. FIG. 23) designedfor storage of medicinal agents within the cold chain. As illustrated inFIG. 1, the structural region 180 may have an attached gas pressuregauge 140, configured to detect and signal the gas pressure within thegas-sealed gap 145. See: Mukugi et al., “Characteristics of cold cathodegauges for outgassing measurements in uhv range,” Vacuum, vol. 44, nos.5-7, 1993, pages 591-593; and Saitoh et al., “Influence of vacuum gaugeson outgassing rate measurements,” Journal of Vacuum Science andTechnology, vol. A11, no. 5, September/October 1993, pages 2816-2821;Hong et al., “Investigation of gas species in a stainless steelultrahigh vacuum chamber with hot cathode ionization gauges,” Meas. Sci.Technol., vol. 15, 2004, pages 359-364; which are each incorporated byreference. The gas pressure gauge 140 may be operably attached to thegas-sealed gap 145 through a tube or duct 175. Although not illustratedin FIG. 1, in some embodiments a valve may be included in or on the duct175 to inhibit the flow of gas through the duct 175 and to isolate thegas-sealed gap 145 from the gas pressure gauge 140.

The structural region 180 fabricated from a heat-sensitive material maybe fabricated from a variety of heat-sensitive materials, depending onthe embodiment. The structural region 180 may be fabricated to include asingle heat-sensitive material. The structural region 180 fabricatedfrom a heat-sensitive material may be fabricated from a plurality ofmaterials, one or more of which may be heat-sensitive, depending on theembodiment. For example, the structural region 180 may be fabricatedpartially or entirely from aluminum. The structural region 180 mayinclude a plurality of materials in a particular embodiment. Thestructural region 180 may be fabricated from composite materials. Forexample, the structural region 180 may be fabricated partially orentirely from metalized plastic, such as polypropylene, PET, nylon orpolyethylene completely covered with a layer of metal, such as aluminum,on the surfaces 190 of the outer wall 150 and the inner wall 155 facingthe gas-sealed gap 145. For example, the structural region 180 may befabricated partially or entirely from plastic with a metal coating, orfrom plastic with a metal liner, on the interior surface of thegas-sealed gap 145 (e.g. as illustrated as surfaces 190 in FIG. 1). Forexample, the structural region 180 may be fabricated partially orentirely from a composite material forming a plastic interior and ametal coating covering the surfaces 190 of the outer wall 150 and theinner wall 155 facing the gas-sealed gap 145. For example, thestructural region 180 may be fabricated partially or entirely from acomposite material forming a plastic interior and a metal liner coveringthe surfaces 190 of the outer wall 150 and the inner wall 155 facing thegas-sealed gap 145. For example, the structural region 180 may befabricated partially or entirely from materials including carbon fibers.The structural region 180 may be fabricated from different materials inlayers or areas of the structural region 180, as suitable for a givenembodiment. For example, the structural region 180 may be fabricatedpartially or entirely from a plastic exterior region with agas-impermeable metal liner covering the surfaces 190 of the outer wall150 and the inner wall 155 facing the gas-sealed gap 145.

In order to maintain a low gas pressure within the gas-sealed gap 145,in some embodiments the structural region 180 is fabricated entirely orpartially from low vapor emitting materials. For example, the structuralregion 180 may be fabricated from low vapor-emitting materials such asaluminum, stainless steel, or other metals. For example, the structuralregion 180 may be fabricated from low vapor-emitting materials such asglass or appropriate ceramics. In order to maintain a low gas pressurewithin the gas-sealed gap 145, in some embodiments the structural region180 is fabricated with a layer of low vapor emitting materials on thesurfaces 190 of the outer wall 150 and the inner wall 155 facing thegas-sealed gap 145. For example, the surfaces 190 may be covered with alayer of stainless steel, aluminum, or other low vapor emittingmaterial. In some embodiments the surfaces 190 of the outer wall 150 andthe inner wall 155 facing the gas-sealed gap 145 is cleaned and treatedprior to assembly to reduce the sublimation of contaminants (e.g. water,oils, or plastics) from the surfaces 190 into the gas-sealed gap 145(see FIG. 5 and associated text herein). The specific type of low vaporemitting material used in the fabrication may be selected based onfactors such as cost, weight, durability, hardness, strength, andanticipated sublimation from the surface of the particular material atthe gas pressures required within the gas-sealed gap 145 and at theexpected temperatures of use in a given embodiment. See, for example,Adams, “A review of the stainless steel surface,” Journal of VacuumScience and Technology, vol. A1, no. 1, January-March 1983, pages 12-18,which is incorporated by reference. For example, in some embodiments amanufactured storage device may include a gas-sealed gap 145 with aninternal gas pressure less than or equal to 1×10⁻² torr. For example, insome embodiments a manufactured storage device may include a gas-sealedgap 145 with an internal gas pressure less than or equal to 5×10⁻⁴ torr.For example, in some embodiments a manufactured storage device mayinclude a gas-sealed gap 145 with an internal gas pressure less than orequal to 1×10⁻² torr. For example, in some embodiments a manufacturedstorage device may include a gas-sealed gap 145 with an internal gaspressure less than or equal to 5×10⁻⁴ torr. For example, in someembodiments a manufactured storage device may include a gas-sealed gap145 with an internal gas pressure less than 1×10⁻² torr, for example,less than 5×10⁻³ torr, less than 5×10⁻⁴ torr, less than 5×10⁻⁵ torr,5×10⁻⁶ torr or 5×10⁻⁷ torr.

The materials used to fabricate the components of the apparatus 185, aswell as any treatment of the components prior to assembly of theapparatus 185 (see, e.g., FIG. 5 and associated text) will influence therate of reduction of gas pressure within the apparatus 185 during thesteps of the methods as described herein (see, e.g., FIGS. 6-22 andassociated text) as well as the maintenance of the low gas pressure overtime. See: R. J. Elsey, “Outgassing of vacuum materials-I,” Vacuum, vol.25, no. 7, 1975, pages 299-306; Yamazake et al., “High-speed pumping toUHV,” Vacuum, vol. 84, 2010, pages 756-759; Saito et al., “Measurementsystem for low outgassing materials by switching between two pumpingpaths,” Vacuum, vol. 47, nos. 6-8, 1996, pages 749-752; Watanabe et al,“Reduction in outgassing rate from residual gas analyzers for extremehigh vacuum measurements,” Journal of Vacuum Science and Technology,vol. A14, no. 6, November/December 1996, pages 3261-3266; Chun et al.,“Effect of the Cr-rich oxide surface on fast pumpdown to ultrahighvacuum,” Journal of Vacuum Science and Technology, vol. A15, no. 5,September/October 1997, pages 2518-2520; and Nemanic and Setina,“Outgassing of a thin wall vacuum insulating panel,” Vacuum, vol. 49,no. 3, 1998, pages 233-237; Poole and Michaelis, “Hiavac and Teflonoutgassing under ultra-high vacuum conditions,” Vacuum, vol. 30, no. 10,1980, pages 415-417; and Ishikawa and Nemanic, “An overview of methodsto suppress hydrogen outgassing rate from austenitic stainless steelwith reference to UHV and EXV,” Vacuum, vol. 69, 2003, pages 501-512;which are each incorporated by reference. The term “outgassing,” as usedherein, refers to the evolution of gas from a solid or liquid in avacuum or low gas pressure environment. See: Redhead, “Recommendedpractices for measuring and reporting outgassing data,” Journal ofVacuum Science and Technology, vol. A20, no. 5, September/October 2002,pages 1667-1675, which is incorporated by reference. The structuralstability and the expected outgassing properties of the materials usedto fabricate the components of the apparatus 185 during expected use ofthe entire apparatus 185 and any independent use of all or part of thestructural region 180 should be taken into account in materialselection. See: S. Choi and B. V. Sankar, “Gas permeability of variousgraphite/epoxy composite laminates for cryogenic storage systems,”Composites: Part B 39, 2008, pages 782-791; Engelmann et al., “Vacuumchambers in composite material,” Journal of Vacuum Science andTechnology, vol. A5, no. 4, July/August 1987, pages 2337-2341; Nemanicand Setina, “Experiments with a thin-walled stainless steel chamber,”Journal of Vacuum Science and Technology, vol. A18, no. 4, July/August2000, pages 1789-1793; Halliday, “An introduction to materials for usein vacuum,” Vacuum, vol. 37, nos. 8/9, pages 583-585, 1987; Holtrop andHansink, “High temperature outgassing test on materials used in DIII-Dtokamak,” Journal of Vacuum Science and Technology, vol. A24, no. 4,July/August 2006, pages 1572-1577; Patrick, “Outgassing and the choiceof materials for space instrumentation,” Vacuum, vol. 23, no. 11, 1973,pages 411-413; Ishimaru, “Ultimate pressure of the order of 10⁻¹³ Torrin an aluminum alloy vacuum chamber,” Journal of Vacuum Science andTechnology, vol. A7, no. 3, May/June 1989, pages 2437-2442; Hirohata etal., “Hydrogen desorption behavior of aluminum materials used forextremely high vacuum chamber,” Journal of Vacuum Science andTechnology, vol. A11, no. 54, September/October 1993, pages 2637-2641;Ishimaru, “Aluminum alloy-sapphire sealed window for ultrahigh vacuum,”Vacuum, vol. 33, no. 6, 1983, pages 339-340; and Nemanic and Setina,“Outgassing in thin wall stainless steel cells,” Journal of VacuumScience and Technology, vol. A17, no. 3, May/June 1999, pages 1040-1046;which are each incorporated by reference. In embodiments whereincomponents of the apparatus 185, such as the connector 120 and/or thestructural region 180, are fabricated from a composite, such as anepoxy-containing material, the outgassing rates and associated weightloss of the components should be taken into account in estimating thetime required to produce a low gas pressure within the apparatus 185using the methods described herein (see, e.g., FIGS. 6-22 and associatedtext). In some situations, materials may sublimate to the extent thattheir structural integrity is reduced at the low gas pressures requiredin a specific embodiment, and such factors should be taken into accountin the design of the apparatus 185 and the structural region 180. See:R. D. Brown, “Outgassing of epoxy resins in vacuum,” Vacuum, vol. 17,no. 9, 1967, pages 505-509; J. Santhanam and P. Vijendran, “Outgassingrate of reinforced epoxy and its control by different pretreatmentmethods,” Vacuum, vol. 28, no. 8/9, 1978, pages 365-366; and Gupta etal., “Outgassing from epoxy resins and methods for its reduction,”Vacuum, vol. 27, no. 2, 1977, pages 61-63, which are each incorporatedby reference.

The term “heat-sensitive,” as used herein, refers to materials that losetheir structural integrity at temperatures below the activationtemperature(s) and under the activation condition(s) for the types ofgetter(s) 110 used in the apparatus 185. The term “heat-sensitive,” asused herein, is relative to the activation temperature(s) and thepressure conditions used for the specific getters 110 included in agiven embodiment. For example, in some embodiments the getters 110included in the apparatus 185 may include zirconium-vanadium-irongetters (see U.S. Pat. No. 4,312,669 “Non-evaporable Ternary GetteringAlloy and Method of Use for the Sorption of Water, Water Vapor and OtherGasses,” to Boffito et al., which is incorporated by reference). Forexample, in some embodiments the getters 110 included in the apparatus185 may include St707™ getters with 70% zirconium, 24.6% vanadium and5.4% iron (for example, available from Getter Technologies InternationalLtd., China). See also Hobson and Chapman, “Pumping of methane by St707at low temperatures,” Journal of Vacuum and Science Technology,” vol.A4, no. 3, May/June 1986, pages 300-302, which is incorporated byreference. As noted in U.S. Pat. No. 4,312,669, ibid., incorporated byreference herein, a zirconium-vanadium-iron getter material may beactivated by heating to a temperature of approximately 700 degreesCentigrade for at least 20 seconds and then reducing the temperature tobetween approximately 400 degrees Centigrade and approximately 25degrees Centigrade. Also as noted in U.S. Pat. No. 4,312,669, ibid.,incorporated by reference herein, a zirconium-vanadium-iron gettermaterial may be activated by heating to a temperature less than 450degrees Centigrade, such as approximately 400 degrees Centigrade, orbetween approximately 250 and approximately 350 degrees Centigrade, fora time between 1 and 10 minutes while in an environment with a gaspressure of less than 10⁻² torr. A “heat-sensitive material,” as usedherein, for use with an embodiment incorporating getters fabricated froma zirconium-vanadium-iron getter material, would be a heat-sensitivematerial that is predicted to lose its structural integrity in atemperature of approximately 700 degrees Centigrade lasting for at least20 seconds. A “heat-sensitive material,” as used herein, for use with anembodiment incorporating getters fabricated from azirconium-vanadium-iron getter material, would lose its structuralintegrity at a temperature less than 450 degrees Centigrade, such asapproximately 400 degrees Centigrade, or between approximately 250 andapproximately 350 degrees Centigrade, for a time between 1 and 10minutes while in an environment with a gas pressure of less than 10⁻²torr. For example, in some embodiments the structural region 180 isfabricated from a heat-sensitive material that includes aluminum, oraluminum alloy that loses its structural integrity at temperatures above250 degrees Centigrade. See: Ishimaru et al., “New all aluminum alloyvacuum system for the TRISTAN e+e− storage accelerator,” IEEETransactions on Nuclear Science, Vol. NS-28, no. 3, 1981, pages3320-3322, which is incorporated by reference.

The term “structural integrity,” as used herein, refers to a structuremaintaining its fabricated form in a set of given conditions. Loss ofstructural integrity, correspondingly, refers to the failure of astructure to maintain its fabricated form in a set of conditions.“Heat-sensitive” materials, as used herein, refers to materials thatlose their structural integrity at temperatures below the activationtemperature(s) and under the activation condition(s) for the types ofgetter(s) 110 used in an embodiment of an apparatus 185. Conditionsaffecting loss of structural integrity may include temperature ranges,such as excessively hot or cold temperatures, and gas pressures, such asminimal gas pressure within an interior region. Conditions affectingloss of structural integrity may include conditions of intended use,such as weight-bearing, erosion, compressive strength, or tensilestrength. Loss of structural integrity may be overt or gross, such aswhen a structure in whole or part melts, deforms, distorts, implodes, orcombusts. Loss of structural integrity may include a change theoutgassing properties of a material used in fabrication of a structure,for example a plastic material with low outgassing properties mayexhibit increased outgassing properties in a set of given conditions,such as temperature or gas pressure. Loss of structural integrity mayalso be inconspicuous or undetectable to a cursory inspection, such asin the formation of a small hole, surface thinning, alteration of acrystalline or other non-overt structure of a fabricated material, orloss of cohesion at a weld or joint. For example, in some embodiments,aluminum and aluminum alloys are “heat-sensitive,” as used herein, andmay lose their structural integrity in some conditions required toactivate some types of getters employed in the specific embodiment. Forexample, although aluminum and aluminum alloys may not completely meltinto a liquid form at temperatures above 250 degrees Centigrade, in someinstances they will begin to soften and, as such, lose their structuralintegrity. Similarly, copper and copper alloys may be consideredheat-sensitive materials in some embodiments. See Koyatsu et al.,“Measurements of outgassing rate from copper and copper alloy chambers,”Vacuum, vol. 47, no. 6-8, 1996, pages 709-711, which is incorporated byreference. When combined with the force of gravity on the structuralregion 180 and any force due to a low gas pressure within the gas-sealedgap 145, aluminum and aluminum alloys at temperatures above 250 degreesCentigrade may lose their structural integrity and manufactured form andcompress, shift, or bend. Similarly, plastic and plastic composites usedin some embodiments may be heat sensitive materials.

As illustrated in FIG. 1, in some embodiments the inner wall 155 and theouter wall 150 of the structural region 180 together substantiallydefine the gas-sealed gap 145. For example, the gas-sealed gap 145 maybe primarily defined by the boundaries of the inner wall 155 and theouter wall 150 of the structural region 180. For example, the gas-sealedgap 145 may be substantially established by the boundaries of the innerwall 155 and the outer wall 150 of the structural region 180. Junctionsbetween the inner wall 155 and the outer wall 150 may be, for example,welds, bonds or seals that substantially isolate the gas-sealed gap 145from the gas environment external to the structural region 180. In someembodiments, the junctions between the inner wall 155 and the outer wall150 may include additional material, such as welding agents, solder,brazing material or other sealing materials to establish and maintainthe isolation of the gas-sealed gap 145 from the gas environmentexternal to the structural region 180.

In some embodiments, the gas-sealed gap 145 includes additionalmaterial. In some embodiments, the gas-sealed gap 145 includesadditional material designed to improve the durability and stability ofthe structural region 180. For example, the gas-sealed gap 145 mayinclude structural features, such as one or more flanges, struts,braces, crossbars, or posts that may be configured to maintain thestability of the structural region 180. For example, the gas-sealed gap145 may include internal support structure, such as reinforced regionsof the inner wall 155 and the outer wall 150.

In some embodiments, the gas-sealed gap 145 includes additionalinsulating material that improves the thermal properties of thestructural region 180. For example, the gas-sealed gap 145 may includemultilayer insulation material (MU). See: Wiedmann et al., “Multi LayerInsulation Literature,” DLR, Institute of Structural Mechanics, 20 pagestotal; Wei et al., “Effects of structure and shape on thermalperformance of perforated multi-layer insulation blankets,” AppliedThermal Engineering, vol. 29, 2009, pages 1264-1266; Halaczek andRafalowicz, “Heat transport in self-pumping multilayer insulation,”Cryogenics, vol. 26, 1986, pages 373-376; Shu et al., “Heat flux from277 to 77 K through a few layers of multilayer insulation,” Cryogenicsvol. 26, 1986, pages 671-677; Jacob et al., “Investigations into thethermal performance of multilayer insulation (300-77 K) Part 1:calorimetric studies,” Cryogenics, vol. 32, no. 12, 1992, pages1137-1146; Jacob et al., “Investigations into the thermal performance ofmultilayer insulation (300-77 K) Part 2: Thermal analysis,” Cryogenics,vol. 32, no. 12, 1992, pages 1147-1153; Halaczek and Rafalowicz,“Unguarded cryostat for thermal conductivity measurements of multilayerinsulations,” Cryogenics, vol. 25, 1985, pages 529-530; Mikhalchenko etal., “Theoretical and experimental investigation of radiative-conductiveheat transfer in multilayer insulation,” Cryogenics, vol. 25, 1985,pages 275-278; Bapat et al., “Experimental investigations of multilayerinsulation,” Cryogenics, vol. 30, 1990, pages 711-719; U.S. Pat. No.5,590,054 to McIntosh, titled “Variable-density method for multi-layerinsulation;” Zhitomirskil et al., “A theoretical model of the heattransfer process in multilayer insulation,” Cryogenics, 1979, pages265-268; Shu, “Systematic study to reduce the effects of cracks inmultilayer insulation Part 1: theoretical model,” Cryogenics, vol. 27,1987, pages 249-256; Shu, “Systematic study to reduce the effects ofcracks in multilayer insulation Part 2: experimental results,”Cryogenics, vol. 27, 1987, pages 298-311; Glassford and Liu, “Outgassingrate of multilayer insulation,” Lockheed Palo Alto Research Laboratory,pages 83-106; Halaczak and Rafalowicz, “Flat-plate cryostat formeasurements of multilayer insulation thermal conductivity,” Cryogenics,vol. 25, 1985, pages 593-595; Matsuda and Yoshikiyo, “Simple structureinsulating material properties for multilayer insulation,” Cryogenics,1980, pages 135-138; Keller et al., “Application of high temperaturemultilayer insulations,” Acta Astronautica, vol. 26, no. 6, 1992, pages451-458; Scurlock and Saull, “Development of multilayer insulations withthermal conductivities below 01. μW cm⁻¹ K⁻¹ ,” Cryogenics, May 1976,pages 303-311; Bapat et al., “Performance prediction of multilayerinsulation,” Cryogenics vol. 30, 1990, pages 700-710; and Kropschot,“Multiple layer insulation for cryogenic applications,” Cryogenics,1961, pages 171-177; which are each incorporated by reference.

In some embodiments, there is at least one section of ultra efficientinsulation material within the gas-sealed gap 145. The term “ultraefficient insulation material,” as used herein, may include one or moretype of insulation material with extremely low heat conductance andextremely low heat radiation transfer between the surfaces of theinsulation material. The ultra efficient insulation material mayinclude, for example, one or more layers of thermally reflective film,high vacuum, aerogel, low thermal conductivity bead-like units,disordered layered crystals, low density solids, or low density foam. Insome embodiments, the ultra efficient insulation material includes oneor more low density solids such as aerogels, such as those described in,for example: Fricke and Emmerling, Aerogels—preparation, properties,applications, Structure and Bonding 77: 37-87 (1992); and Pekala,Organic aerogels from the polycondensation of resorcinol withformaldehyde, Journal of Materials Science 24: 3221-3227 (1989), whichare each herein incorporated by reference. As used herein, “low density”may include materials with density from about 0.01 g/cm³ to about 0.10g/cm³, and materials with density from about 0.005 g/cm³ to about 0.05g/cm³. In some embodiments, the ultra efficient insulation materialincludes one or more layers of disordered layered crystals, such asthose described in, for example: Chiritescu et al., Ultralow thermalconductivity in disordered, layered WSe₂ crystals, Science 315: 351-353(2007), which is herein incorporated by reference. In some embodiments,the ultra efficient insulation material includes at least two layers ofthermal reflective film surrounded, for example, by at least one of:high vacuum, low thermal conductivity spacer units, low thermalconductivity bead like units, or low density foam. See, for example,Mikhalchenko et al., “Study of heat transfer in multilayer insulationbased on composite spacer materials,” Cryogenics, 1983, pages 309-311,which is incorporated by reference herein. In some embodiments, theultra efficient insulation material may include at least two layers ofthermal reflective material and at least one spacer unit between thelayers of thermal reflective material. For example, the ultra-efficientinsulation material may include at least one multiple layer insulatingcomposite such as described in U.S. Pat. No. 6,485,805 to Smith et al.,titled “Multilayer insulation composite,” which is herein incorporatedby reference. For example, the ultra-efficient insulation material mayinclude at least one metallic sheet insulation system, such as thatdescribed in U.S. Pat. No. 5,915,283 to Reed et al., titled “Metallicsheet insulation system,” which is herein incorporated by reference. Forexample, the ultra-efficient insulation material may include at leastone thermal insulation system, such as that described in U.S. Pat. No.6,967,051 to Augustynowicz et al., titled “Thermal insulation systems,”which is herein incorporated by reference. For example, theultra-efficient insulation material may include at least one rigidmultilayer material for thermal insulation, such as that described inU.S. Pat. No. 7,001,656 to Maignan et al., titled “Rigid multilayermaterial for thermal insulation,” which is herein incorporated byreference. See also: Li et al., “Study on effect of liquid level on theheat leak into vertical cryogenic vessels,” Cryogenics, vol. 50, 2010,pages 367-372; Barth et al., “Test results for a high quality industrialsuperinsulation,” Cryogenics, vol. 28, 1988, pages 607-609; and Eyssaand Okasha, “Thermodynamic optimization of thermal radiation shields fora cryogenic apparatus,” Cryogenics, 1978, pages 305-307; which are eachincorporated by reference. For example, the ultra-efficient insulationmaterial may include multilayer insulation material, or “MLI.” Forexample, an ultra efficient insulation material may include multilayerinsulation material such as that used in space program launch vehicles,including by NASA. See, e.g., Daryabeigi, Thermal analysis and designoptimization of multilayer insulation for reentry aerodynamic heating,Journal of Spacecraft and Rockets 39: 509-514 (2002), which is hereinincorporated by reference. For example, the ultra efficient insulationmaterial may include space with a gaseous pressure lower thanatmospheric pressure external to the gas-sealed gap 145. See, forexample, Nemanic, “Vacuum insulating panel,” Vacuum, vol. 46, nos. 8-10,1995, pages 839-842, which is incorporated by reference. In someembodiments, the ultra efficient insulation material may substantiallycover the inner wall 155 surface facing the gas-sealed gap 145. In someembodiments, the ultra efficient insulation material may substantiallycover the outer wall 150 surface facing the gas-sealed gap 145.

In some embodiments, there is at least one layer of multilayerinsulation material (“MLI”) within the gas-sealed gap 145. The at leastone layer of multilayer insulation material may substantially surroundthe surface of the inner wall 155. In some embodiments, there are aplurality of layers of multilayer insulation material within thegas-sealed gap 145, wherein the layers may not be homogeneous. Forexample, the plurality of layers of multilayer insulation material mayinclude layers of differing thicknesses, or layers with and withoutassociated spacing elements. In some embodiments there may be one ormore additional layers within or in addition to the insulation material,such as, for example, an outer structural layer or an inner structurallayer. An inner or an outer structural layer may be made of any materialappropriate to the embodiment, for example an inner or an outerstructural layer may include: plastic, metal, alloy, composite, orglass. See, for example, U.S. Pat. No. 4,726,974 to Nowobilski et al.,titled “Vacuum insulation panel,” which is incorporated by reference. Insome embodiments, there may be one or more layers of high vacuum betweenlayers of thermal reflective film. In some embodiments, the gas-sealedgap 145 includes a substantially evacuated gaseous pressure relative tothe atmospheric pressure external to the structural region 180. Asubstantially evacuated gaseous pressure relative to the atmosphericpressure external to the structural region 180 may include substantiallyevacuated gaseous pressure surrounding a plurality of layers of MLI, forexample between and around the layers. A substantially evacuated gaseouspressure relative to the atmospheric pressure external to the structuralregion 180 may include substantially evacuated gaseous pressure in oneor more sections of the gas-sealed gap 145. For example, in someembodiments the gas-sealed gap 145 includes substantially evacuatedspace having a pressure less than or equal to 1×10⁻² torr. For example,in some embodiments the gas-sealed gap 145 includes substantiallyevacuated space having a pressure less than or equal to 5×10⁻⁴ torr. Forexample, in some embodiments the gas-sealed gap 145 includessubstantially evacuated space having a pressure less than or equal to1×10⁻² torr in the gas-sealed gap 145. For example, in some embodimentsthe gas-sealed gap 145 includes substantially evacuated space having apressure less than or equal to 5×10⁻⁴ torr in the gas-sealed gap 145. Insome embodiments, the gas-sealed gap 145 includes substantiallyevacuated space having a pressure less than 1×10⁻² torr, for example,less than 5×10⁻³ torr, less than 5×10⁻⁴ torr, less than 5×10⁻⁵ torr,less than 5×10⁻⁶ torr or less than 5×10⁻⁷ torr. For example, in someembodiments the gas-sealed gap 145 includes a plurality of layers ofmultilayer insulation material and substantially evacuated space havinga pressure less than or equal to 1×10⁻² torr. For example, in someembodiments the gas-sealed gap 145 includes a plurality of layers ofmultilayer insulation material and substantially evacuated space havinga pressure less than or equal to 5×10⁻⁴ torr.

As illustrated in FIG. 1, during some steps of the methods describedherein, and when included with the apparatus 185, the gas-sealed gap 145of the structural region 180 is open to the interior of the connector120. The structural region 180 is joined to the connector 120 in amanner to form a substantially gas sealed space with the interior of thegas-sealed gap 145. The structural region 180 is operably attached tothe connector 120 with a seal sufficient to maintain low gas pressurewithin the gas-sealed gap 145, such as through action of the vacuum pump130. The structural region 180 is operably attached to the connector 120with a seal sufficient to maintain minimal gas pressure within thegas-sealed gap 145, such as through action of the vacuum pump 130. Forexample, the structural region 180 may be operably attached to theconnector 120 with a seal sufficient to maintain gas pressure less thanor equal to 1×10⁻² torr within the gas-sealed gap 145 through action ofthe vacuum pump 130. As illustrated in FIG. 1, some embodiments mayinclude a valve 135 integral to the connector 120 and adjacent to theouter wall 150 of the structural region 180, wherein the valve 135 isoperably attached in an orientation to isolate the interior of theconnector 120 on the opposing ends of the valve 135.

The apparatus 185 includes an activation region 100 fabricated from aheat-resistant material, the activation region 100 including one or moregetters 110. Although a single activation region 100 is depicted inFIGS. 1-4, in some embodiments there may be a plurality of activationregions that may be fabricated from the same or different heat-resistantmaterials and may contain either the same or different types of getters.In embodiments with a plurality of activation regions, each region maybe independently operably attached to a connector. In embodiments with aplurality of activation regions, there may be one or more valvesoperably attached between one or more of the plurality of activationregions and the associated connector.

As used herein, the term “heat-resistant material” refers to materialsthat maintain their structural integrity at temperatures and conditionsabove the activation temperature(s) and within the condition(s) for thetypes of getter(s) 110 used in the apparatus 185. The term“heat-resistant,” as used herein, is relative to the activationtemperature(s) and gas pressure conditions used for the specific getters110 included in a given embodiment. For example, in some embodiments thegetters 110 included in the apparatus 185 may includezirconium-vanadium-iron getters (see U.S. Pat. No. 4,312,669, ibid.,incorporated by reference herein). For example, in some embodiments thegetters 110 included in the apparatus 185 may include St707™ getterswith 70% zirconium, 24.6% vanadium and 5.4% iron (for example, availablefrom Getter Technologies International Ltd., China). See: Gunter et al.,“Microstructure and bulk reactivity of the nonevaporable getterZr₅₇V₃₆Fe₇ ,” Journal of Vacuum Science Technology, Vol. A16, no. 6,November/December 1998, pages 3526-3535, which is incorporated byreference. As noted in U.S. Pat. No. 4,312,669, ibid., incorporated byreference herein, a zirconium-vanadium-iron getter material may beactivated by heating to a temperature of approximately 700 degreesCentigrade for at least 20 seconds and then reducing the temperature tobetween approximately 400 degrees Centigrade and approximately 25degrees Centigrade. Also as noted in U.S. Pat. No. 4,312,669, ibid.,incorporated by reference herein, a zirconium-vanadium-iron gettermaterial may be activated by heating to a temperature less than 450degrees Centigrade, such as approximately 400 degrees Centigrade, orbetween approximately 250 and approximately 350 degrees Centigrade, fora time between 1 and 10 minutes while in an environment with a gaspressure of less than 10⁻² torr. A “heat-resistant material,” as usedherein, for use with an embodiment incorporating getters fabricated froma zirconium-vanadium-iron getter material, would be a heat-resistantmaterial that is predicted to maintain its structural integrity in atemperature of approximately 700 degrees Centigrade lasting for at least20 seconds. A “heat-resistant material,” as used herein, for use with anembodiment incorporating getters fabricated from azirconium-vanadium-iron getter material, would conserve its structuralintegrity at a temperature less than 450 degrees Centigrade, such asapproximately 400 degrees Centigrade, or between approximately 250 andapproximately 350 degrees Centigrade, for a time between 1 and 10minutes while in an environment with a gas pressure of less than 10⁻²torr. For example, in some embodiments the getters 110 included in theapparatus 185 may include getters fabricated from atitanium-zirconium-vanadium getter material. See: Matolin and Johanek,“Static SIMS study of TiZrV NEG activation,” Vacuum, vol. 67, 2002,pages 177-184, which is incorporated by reference. A “heat-resistantmaterial,” as used herein, for use with an embodiment incorporatinggetters fabricated from a titanium-zirconium-vanadium getter material,would conserve its structural integrity at a temperature less ofapproximately 300 degrees Centigrade with a gas pressure within theinterior of approximately 5×10⁻¹¹ mbar (see Matolin and Johanek, ibid,which is incorporated by reference). For example, in some embodimentsthe structural region 180 is fabricated from a heat-resistant materialthat includes stainless steel, or stainless steel alloys. For example,in some embodiments the structural region 180 is fabricated from aheat-resistant material that includes titanium alloy.

Getters of a variety of types may be used in different embodiments. Thegetters may be fabricated from a variety of getter materials. Forexample, the getters may be fabricated from non-evaporatable gettermaterial. The selection of getters may depend, for example, on theavailability, cost, mass, chemical composition, toxicity and durabilityof the getter material employed in a given embodiment. The selection ofgetters may depend, for example, on the activation temperature andconditions for a particular getter material. Some types of getters areactivatable at different temperatures and gas pressure conditions fordifferent lengths of time (see, e.g. U.S. Pat. No. 4,312,669“Non-evaporable Ternary Gettering Alloy and Method of Use for theSorption of Water, Water Vapor and Other Gasses,” to Boffito et al.,which is incorporated by reference), and for such getter materials theselection of the materials may depend on the range of potentialtemperatures, gas pressure conditions, and times, or one or morecombinations of activation temperatures, gas pressure conditions andtimes for a specific getter material. Some getters may require gaspressure conditions less than atmospheric pressures, such as near-vacuumconditions, during activation at particular temperatures (see Matolinand Johanek, ibid, and U.S. Pat. No. 4,312,669, ibid., which are eachincorporated by reference). The selection of getters may depend, forexample, on the operational temperature of a given getter material, suchas within ambient temperatures (i.e. substantially between 20 degreesCentigrade and 30 degrees Centigrade), within refrigeration temperatures(i.e. substantially between 2 degrees Centigrade and 10 degreesCentigrade) or within freezing temperatures (for example, substantiallybetween 0 degrees Centigrade and −10 degrees Centigrade, orsubstantially between −15 degrees Centigrade and −25 degreesCentigrade). Some embodiments may include a single type of getters, forexample getters fabricated from substantially the same active gettermaterial. Some embodiments may include a plurality of types of gettersfabricated from substantially distinct getter materials. Moreinformation regarding types of getters and getter materials suitable forvarious embodiments of the invention may be found in: Tripathi et al.,“Hydrogen intake capacity of ZrVFe alloy bulk getters,” Vacuum, vol. 48,no. 12, 1997, pages 1023-1025; Benvenuti et al., “Nonevaporable getterfilms for ultrahigh vacuum applications,” Journal of Vacuum and ScienceTechnology, vol. A16, no. 1, January/February 1998, pages 148-154;Benvenuti et al., “Decreasing surface outgassing by thin film gettercoatings,” Vacuum, vol. 50, nos. 1-2, 1998, pages 57-63; Boffito et al.,“A nonevaporable low temperature activatable getter material,” Journalof Vacuum and Science Technology, vol. 18, no. 3, May/June 1981, pages1117-1120; della Porta, “Gas problem and gettering in sealed-off vacuumdevices,” Vacuum, vol. 47, nos 6-8, 1996, pages 771-777; Benvenuti andChiggiato, “Obtention of pressures in the 10-14 torr range by means of aZr—V—Fe non evaporable getter,” Vacuum, vol. 44, nos. 5-7, 1993, pages511-513; Londer et al., “New high capacity getter for vacuum insulatedmobile LH₂ storage tank systems,” Vacuum, vol. 82, 2008, pages 431-434;Li et al., “Design and pumping characteristics of a compacttitanium-vanadium non-evaporable getter pump,” Journal of Vacuum andScience Technology, vol. A16, no. 3, May/June 1998, pages 1139-1144;Chiggiato, “Production of extreme high vacuum with non evaporablegetters,” Physica Scripta, vol. T71, 1997, pages 9-13; Benvenuit andChiaggiato, “Pumping characteristics of the St707 nonevaporable getter(Zr 70 V 24.6-Fe 5.4 wt %),” Journal of Vacuum and Science Technology,vol. A14, no. 6, November/December 1996, pages 3278-3282; Day, “The useof active carbons as cryosorbent,” Colloids and Surfaces A: Physicochem.Eng. Aspects 187-188, 2001, pages 187-206; U.S. Pat. No. 4,312,669“Non-evaporable Ternary Gettering Alloy and Method of Use for theSorption of Water, Water Vapor and Other Gasses,” to Boffito et al.;Hobson and Chapman, “Pumping of methane by St707 at low temperatures,”Journal of Vacuum and Science Technology, vol. A4, no. 3, May/June 1986,pages 300-302; and Matolin and Johanek, “Static SIMS study of TiZrV NEGactivation,” Vacuum, vol. 67, 2002, pages 177-184; which are eachincorporated by reference.

As illustrated in FIG. 1, the activation region 100 includes wallsforming a gas-sealed interior. The gas-sealed interior of the activationregion 100 encloses one or more getters 110. Also as illustrated in FIG.1, the activation region 100 includes a gas-sealed interior enclosingone or more getters 110, wherein the gas-sealed interior of theactivation region 100 is open to the interior of the connector 120. Thegas-sealed interior of the activation region 100 is configured tomaintain a reduced gas pressure as established by the vacuum pump 130.Although not illustrated in FIG. 1, some embodiments may include a valve(e.g. as valve 135) located integral to the connector 120 at a locationadjacent to the activation region 100, the valve configured to isolatethe gas pressure within the connector 120 at the opposite sides of thevalve.

As noted herein, the apparatus 185 is configured to establish andmaintain a reduced gas pressure environment within the gas-sealed gap145 of the structural region 180. Accordingly, the one or more getters110 may include non-evaporatable getter material. The one or moregetters 110 may include zirconium, vanadium and iron. For example, theone or more getters 110 may include 70% zirconium, 24.6% vanadium and5.4% iron. For example, the one or more getters 110 may include St707getters (available, for example, from SAES Getters Group, with corporateheadquarters in Lainate, Italy; see attached online brochure downloadedon Sep. 21, 2011, which is incorporated by reference herein). Similargetter materials are also available from other sources, such as GetterTechnologies International Ltd., China.

As illustrated in FIG. 1, the apparatus 185 includes a connector 120attached to the structural region 180 and to the activation region 100,the connector 120 including a flexible region 125 and a region 127configured for sealing and detachment of the structural region 180 fromthe activation region 100. The connector 120 may be fabricated, forexample, from stainless steel or stainless steel alloy. The connector120 may be fabricated, for example, from different materials indifferent regions, as appropriate to the embodiment. Generally, theconnector 120 is fabricated from material(s) with low vapor emission onthe surface within the connector 120 as well as sufficient strength,durability, and heat tolerance for a specific embodiment and associatedmethods (as described further in the section below). Cost, weight, andflexibility may also be factors in the selection of material(s) forfabrication of the connector 120. See, for example, Nemanic and Setina,“A study of thermal treatment procedures to reduce hydrogen outgassingrate in thin wall stainless steel cells,” Vacuum, vol. 53, 1999, pages277-280; and Koyatsu et al., “Measurements of outgassing rate fromcopper and copper alloy chambers,” Vacuum, vol. 47, no. 6-8, 1996, pages709-711, which are each incorporated by reference.

The connector may include a valve 135 configured to inhibit the flow ofgas within the connector 120. Some embodiments may include more than onevalve. As illustrated in FIG. 1, a valve 135 may be operably attached tothe connector 120 at a location between the vacuum pump 130 and theouter wall 150 of the structural region. The valve 135 may be operablyattached to the connector 120 at a location between the vacuum pump 130and the region 127 configured for sealing and detachment of thestructural region 180 from the activation region 100.

As illustrated in FIG. 1, in some embodiments the flexible region 125 ofthe connector 120 is adjacent to the activation region 100 of theapparatus 185. The flexible region 125 is configured to allow theactivation region 100 to shift orientation relative to the remainder ofthe apparatus 185 (see also FIGS. 2-4) while retaining the low gaspressure within the connector as established and maintained by thevacuum pump 130. As illustrated in FIG. 1, the flexible region 125 isconfigured in an arc forming approximately a right angle, with theresult that the activation region 100 and the structural region 180 arenot in a horizontally linear alignment. As illustrated in FIGS. 1-4, insome embodiments the flexible region 125 of the connector 120 isconfigured to flex along the long axis of the connector 120 (i.e. asdepicted by the double headed arrow in FIG. 1). The change inconfiguration of the flexible region 125 results in the change inrelative orientation of the activation region 100 and the structuralregion 180, as illustrated in FIGS. 1-4. The flexible region 125 may beflexible due to the combination of the material from which it isfabricated as well as the configuration of that material. For example,the flexible region 125 of the connector 120 may be fabricated fromstainless steel in a bellows-type configuration. A bellows-typeconfiguration would be fabricated from suitable material and configuredto allow for flexibility in the flexible region 125 of the connector120. For example, the flexible region 125 of the connector 120 may befabricated from stainless steel and configured in a corrugated,channeled, grooved or ridged shape to allow for flexibility of theflexible region 125 of the connector 120.

As illustrated in FIG. 1, the apparatus 185 includes a vacuum pump 130operably attached to the connector 120. The vacuum pump 130 hassufficient pumping strength to establish a gas pressure within theapparatus 185 less than the gas pressure in the environment adjacent tothe apparatus 185. In some embodiments, the vacuum pump 130 hassufficient pumping strength to establish a gas pressure that issubstantially evacuated. In some embodiments, the vacuum pump 130 hassufficient pumping strength to establish a gas pressure that is nearvacuum. For example, in some embodiments the vacuum pump 130 hassufficient pumping strength to evacuate the gas-sealed gap 145 in theinterior of the structural region 180, the interior of the activationregion 100 and the interior of the connector 120 to a gas pressure lessthan or equal to 1×10⁻² torr. For example, in some embodiments thevacuum pump 130 has sufficient pumping strength to evacuate thegas-sealed gap 145 in the interior of the structural region 180, theinterior of the activation region 100 and the interior of the connector120 to a gas pressure less than or equal to 5×10⁻³ torr, 5×10⁻⁴ torr,5×10⁻⁵ torr, 5×10⁻⁶ torr or 5×10⁻⁷ torr. The vacuum pump 130 may be arotary vane style vacuum pump. Suitable vacuum pumps for someembodiments are manufactured, for example, by Pfeiffer Balzers Company,(Pfeiffer Vacuum GmbH, Germany). Suitable vacuum pumps for someembodiments are manufactured, for example, by the Edwards Vacuum Company(US Headquarters Tewksbury Mass.; Global Headquarters United Kingdom).Vacuum pumps suitable in some embodiments include Pfeiffer Balzers modelTSH060 and Edwards model RV12.

The apparatus 185 includes a region 127 of the connector 120 configuredfor sealing and detachment of the structural region 180 from theactivation region 100. In some embodiments, the apparatus 185 includes aregion 127 of the connector 120 configured for sealing and detachment ofthe connector 120 adjacent to the structural region 180 along the lengthof the connector 120. As illustrated in FIG. 1, the region 127 of theconnector 120 configured for sealing and detachment of the structuralregion 180 from the remainder of the apparatus 185 may be located in aregion of the connector 120 adjacent to the outer wall 150 of thestructural region 180. The apparatus 185 includes a region 127 of theconnector 120 configured for sealing and detachment configured to allowfor the gas-sealed gap 145 within the structural region 180 to maintainits low gas pressure (e.g. less than or equal to 1×10⁻² torr) duringdetachment of the structural region 180 from the remainder of theapparatus 185. The region 127 of the connector 120 configured forsealing and detachment of the structural region 180 from the activationregion 100 may be, for example, a section of aluminum tubing. Inembodiments using aluminum tubing for the region 127 of the connector120 configured for sealing and detachment of the structural region 180from the activation region 100, the aluminum tube may be, for example,one half inch in diameter and 0.035 inches thick tubing, such as model3003-O available from Aircraft Spruce and Specialty Company (Corona,Calif.). In embodiments including aluminum tubing for the region 127 ofthe connector 120 configured for sealing and detachment of thestructural region 180 from the activation region 100, the aluminum tubemay be, for example, collapsed on itself (i.e. “pinched off”) and theedges sealed together using a pinch and crimp instrument. For example,an ultrasonic welder may be used to seal and detach the sections ofaluminum tubing.

The apparatus 185, as illustrated in FIGS. 1-4 and as described in theassociated methods herein, is designed and fabricated to allow activatedgetters 110 to be moved within the apparatus 185 from the activationregion 100 through the connector 120 into the gas-sealed gap 145 withinthe structural region 180. The activated getters 110 are moved withinthe apparatus 185 while the interior spaces of the activation region100, the connector 120 and the gas-sealed gap 145 within the structuralregion 180 include gas pressure lower than that in the environmentsurrounding the apparatus 185. The activated getters 110 are movedwithin the apparatus 185 while the interior spaces of the activationregion 100, the connector 120 and the gas-sealed gap 145 within thestructural region 180 are being actively evacuated by the vacuum pump130. Further aspects of the apparatus 185 are shown in FIGS. 2-4. FIGS.2-4 illustrate additional aspects of the apparatus 185 shown in FIG. 1,particularly in relation to the design and fabrication of the apparatus185 to allow the activated getters 110 to move within the interior ofthe connector 120 between the activation region 100 and the gas-sealedgap 145.

FIG. 2 depicts the apparatus 185 with the flexible region 125 of theconnector 120 moved so that the activation region 100 is directly abovethe structural region 180. As shown in FIG. 2, the flexible region 125of the connector 120 is fabricated and configured to allow it to bendinto a substantially straight configuration. As is apparent from thecombination of FIGS. 1 and 2, the flexible region 125 of the connector120 is fabricated and configured to allow it to bend from asubstantially right angle (as shown in FIG. 1) to a substantially linearconfiguration (as shown in FIG. 2). This motion is depicted by thedouble-headed arrow in FIG. 2. The apparatus 185 depicted in FIG. 2 isoriented with the flexible region 125 of the connector 120 so that theactivation region 100 is directly above the structural region 180 toallow for the getters 110 A, 110 B, 110 C, to fall with the force ofgravity (depicted by the single headed arrows) through the connector 120and into the gas-sealed gap 145.

FIG. 2 also depicts the motion of the activated getters 110 A, 110 B,110 C, from the activation region 100 through the connector 120 (e.g.illustrated with single-headed arrows). For purposes of illustration,the getters 110 as shown in FIG. 1 are given individual identifiers A, Band C in FIG. 2; however, the individual getters 110 A, 110 B, 110 C areintended to be equivalent to the group of getters 110 shown in FIGS. 1,3, 4 and 5. Although three individual getters 110 A, 110 B, 110 C in asubstantially oval shape are shown, the specific number and shape of thegetters 110 would depend on the specific embodiment. As illustrated inFIG. 2, the apparatus 185 is fabricated from material configured toallow the getters 110 A, 110 B, 110 C to move from the activation region100 through the connector 120. The getters 110 selected for a particularembodiment should be of a size and shape to move out of the activationregion 100, through the connector 120, and into the gas-sealed gap 145of the structural region 180. Getters in a form with rounded edges arewell-suited for this purpose, but getters of varying shapes may be usedin different embodiments. Getters formed as granules may be utilized insome embodiments, however getters formed as granular shapes may becomestuck within the connector 120 and not move easily into the gas-sealedgap 145. Preferably, the entirety of the getters 110 should be locatedwithin the gas-sealed gap 145 at the end of the method steps.Preferably, no getters 110 should remain in the connector 120 duringsealing of the connector 120. For example, the getter material mayreduce the integrity of the sealed region of the connector 120.

Correspondingly, the activation region 100 should be operably attachedto the connector 120 in a manner to minimally impede the movement of thegetters 110 out of the activation region 100 and into the internalregion within the connector 120. The attachment should provide asufficient seal to allow for the establishment and maintenance of areduced gas pressure (e.g. less than or equal to 1×10⁻² torr) within theinterior of the apparatus 185 by the vacuum pump 130. For example, inembodiments where the apparatus is fabricated from metal, the activationregion 100 may be attached to the connector 120 by weld junctions. Theseweld junctions should be sufficiently smooth and minimally facing on theinterior of the apparatus 185 to provide minimal impedance of thegetters 110 through the connector 120. Similarly, the structural region180 should be operably attached to the connector 120 in a manner tominimally impede the movement of the getters 110 out of the interior ofthe connector 120 and into the gas-sealed gap 145 within the structuralregion 180.

The interior diameter of the connector 120, including within its ownregions 125 and 127, as well as the interior diameter of any valve(s)(e.g. 135) opening(s) should be suitable for the passage of the getters110 through the apparatus 185 between the activation region 100 and thegas-sealed gap 145 in the structural region 180. The size and shape ofany particular getters 110 used should be less than the interiordiameter of the connector 120 and any valve(s) (e.g. 135) utilizedwithin the apparatus 185. The interior of the connector 120 and anyvalve(s) (e.g. 135) incorporated into the apparatus 185 should includeminimal surfaces which may impede the movement of the getters 110through the apparatus 185. For example, the interior of the connector120 and any valve(s) (e.g. 135) should be substantially smooth, withoutsharp, jutting, or rough edges that may impede the getters 110. Forexample, the interior of the connector 120 and any valve(s) (e.g. 135)should be substantially free of internal elements, such as struts orbraces, which may inhibit getters 110 travelling through the interior.Generally, the interior of the apparatus 185 should be designed andfabricated to allow for the direct movement of the getters 110 from theinterior of the activation region 100 through the connector 120 and intothe gas-sealed gap 145 in the structural region 180 when the activationregion 100, connector 120 and the structural region 180 areappropriately oriented (i.e. as depicted in FIG. 2). In someembodiments, the interior of the apparatus 185 should be designed andfabricated to allow for the direct movement of the getters 110 from theinterior of the activation region 100 through the connector 120 and intothe gas-sealed gap 145 in the structural region 180, such as through theforce of gravity, when the activation region 100, connector 120 and thestructural region 180 are appropriately positioned (i.e. as depicted inFIG. 2). In some embodiments, the interior of the apparatus 185 shouldbe designed and fabricated to allow for the direct movement of thegetters 110 through mechanical transfer from the interior of theactivation region 100 through the connector 120 and into the gas-sealedgap 145 in the structural region 180.

FIG. 2 depicts the flexible region 125 of the connector 120 in asubstantially straight configuration, and with the activation region 100of the apparatus 185 positioned above the structural region 180. Theapparatus is fabricated to allow the flexible region 125 of theconnector to move the relative positioning of the apparatus 185, asillustrated in the double-headed arrow, between the position shown inFIG. 1 and that shown in FIG. 2. FIG. 2 depicts getter 110 A in aposition to soon fall through the force of gravity (depicted by downwardfacing arrows) through the connector 120 and into the gas-sealed gap 145of the structural region 180. FIG. 2 also depicts getter 110 Bpositioned within the connector 120 and moving through the force ofgravity through the connector 120 towards the structural region 180.FIG. 2 depicts getter 110 C in the junction between the gas-sealed gap145 of the structural region 180 and the connector 120 adjacent to theouter wall 150.

FIG. 3 illustrates the apparatus 185 positioned similarly to that shownin FIG. 2, at a later stage (see methods described herein). In the viewillustrated in FIG. 3, the activated getters 110 are all positionedwithin the gas-sealed gap 145 of the structural region 180. Although theactivated getters 110 are illustrated in a cluster in FIG. 3, they mayalso be distributed within the gas-sealed gap 145. In some embodiments,structural elements within the gas-sealed gap 145 confine some or all ofthe activated getters 110 into a defined region of the gas-sealed gap145. For example, the gas-sealed gap 145 may include internal braces orstruts that restrict the mobility of the getters 110 within thegas-sealed gap 145. For example, the gas-sealed gap 145 may include wirenetting material configured to restrict the movement of the getters 110within the gas-sealed gap 145.

FIG. 3 depicts that the connector 120 includes a crimped area 300 withthe opposing faces of the connector brought together to form agas-impermeable seal. The crimped area 300 is within the region 127configured for sealing and detachment of the connector 120. As shown inFIG. 3, the crimped area 300 may be positioned adjacent to the outerwall 150 of the structural region 180, but with a length 320 of theconnector 120 between the crimped area 300 and the surface of the outerwall 150. Also as shown in FIG. 3, there may be a length 310 of theconnector 120 between the crimped area 300 and a valve 135. Asillustrated by the double-headed arrows in FIG. 3, after the crimpedarea 300 is formed, the structural region 180 is detached from theremainder of the apparatus 185. In order to detach the structural region180 from the remainder of the apparatus 185, the connector 120 isseparated at the crimped area while maintaining the reduced gas pressure(e.g. less than or equal to 1×10⁻² torr) within the gas-sealed gap 145.In some embodiments, a gas-impermeable seal may be formed in theconnector 120 substantially simultaneously as the separation at thesealed site. For example, the connector 120 may be sealed and separatedwith an ultrasonic welding device.

FIG. 4 shows the apparatus 185 positioned similarly to that shown inFIG. 3, at a later stage (see methods described herein). In FIG. 4, theactivated getters 110 are within the gas-sealed gap 145. Also as shownin FIG. 4, the connector 120 has been separated at the crimped area 300.The separation of the connector 120 at the crimped area 300 results inthe detachment of the structural region 180 from the remainder of theapparatus 185 (double headed arrows). FIG. 4 also shows a sealing agent400 applied to the surface of the crimped area 300 adjacent to thestructural region 180. The sealing agent 400 is positioned and appliedto ensure that the crimped area 300 adjacent to the structural region180 maintains its structural integrity and does not include any holes orspaces that would permit gas from the environment external to the outerwall 150 to enter the gas-sealed gap 145. The sealing agent 400, ifincluded in a particular embodiment, adheres to the surface of theseparated crimped area 300 to form a gas-tight seal on the interior ofthe connector length 310 adjacent to the outer wall 150. For example,the sealing agent may include epoxy material.

FIG. 23 depicts a cross-section view of a substantially thermally sealedstorage container, such as may be included in a structural region 180 ofan apparatus (not depicted in FIG. 23). The cross-section view ispresented to illustrate various aspects of the container that are notvisible in an external view. The cross-section presented isapproximately half of the container, with the omitted region beingsubstantially similar to the illustrated region. FIG. 23 is an exampleof an embodiment of a unit included in a structural region 180 of anapparatus (not depicted in FIG. 23), although other embodiments arewithin the scope of the disclosure herein. The substantially thermallysealed storage container depicted in FIG. 23 includes an outer wall 150and an inner wall 155. The inner wall 155 substantially defines astorage region 165 within the container. The outer wall 150 and theinner wall 155 are separated by a gas-sealed gap 145.

The container depicted in FIG. 23 also includes an access tube 2340between the interior storage region 165 and the exterior of thecontainer. The access tube 2340 is attached to the inner wall 155 with agas-impermeable seal 2320. For example, the access tube 2340 and theinner wall 155 may both be fabricated from stainless steel, and thegas-impermeable seal 2320 may be a suitable weld joint. The interior ofthe access tube 2340 forms an opening 160 between the exterior of thecontainer and the interior storage region 165. The opening 160 is of asufficient size and shape to allow stored material to be placed withinand removed from the interior of the interior storage region 165, whilesubstantially maintaining the storage and thermal properties of theinterior storage region 165. The container also includes a neck region2330 in a substantially tubular structure surrounding the access tube2340. The neck region 2330 is attached to the outer wall 150 with agas-impermeable seal 2360. For example, the neck region 2330 and theouter wall 150 may both be fabricated from stainless steel, and thegas-impermeable seal 2360 may be a suitable weld joint. The end of theaccess tube 2340 distal to the inner wall 155 and the end of the neckregion 2330 distal to the outer wall 150 are connected with an end seal2310. Although the end seal 2310 depicted is a discrete unit joining thegap between the surfaces of the access tube 2340 and the neck region2330, the end seal 2310 may also include a crimp or other form of agas-impermeable seal. As shown in FIG. 23, the gas-sealed gap 145 may becoextensive with the region 2350 between the neck region 2330 and theaccess tube 2340.

FIG. 23 also depicts two ducts 175 attached to the outer wall 150. Theseducts 175 may be suitable for the attachment of a gas pressure gauge(such as identified as 140 in FIGS. 1-4) or other device as suitable tothe embodiment. In the embodiment illustrated in FIG. 23, the ends ofthe ducts 175 are closed with barrier units 2300 secured with agas-impermeable seal, such as welds or rivets. As the ducts 175 arecoextensive with the gas-sealed gap 145, the ducts 175 should besimilarly gas-sealed to preserve the reduced gas pressure (e.g. lessthan or equal to 1×10⁻² torr) within the gas-sealed gap 145.

A storage container such as depicted in FIG. 23 may include phase-changematerial within the interior storage region 165. Generally speaking,specific properties of the materials, including durability, mass,corrosiveness, toxicity, and cost, should be taken into account in theselection of the materials used in fabricating a storage container. See,for example, Nemanic and Setina, “A study of thermal treatmentprocedures to reduce hydrogen outgassing rate in thin wall stainlesssteel cells,” Vacuum, vol. 53, 1999, pages 277-280; and Koyatsu et al.,“Measurements of outgassing rate from copper and copper alloy chambers,”Vacuum, vol. 47, no. 6-8, 1996, pages 709-711, which are eachincorporated by reference. In embodiments including phase changematerials, the specific properties of the phase change materials,including durability, mass, corrosiveness, toxicity, and cost, should betaken into account in the selection of the materials used in fabricatingthe storage container. For example, the inner wall 155 should befabricated from a material that retains its structural stability in thepresence of the specific phase change material utilized under theexpected use conditions. See: Zalba et al., “Review on thermal energystorage with phase change: materials, heat transfer analysis andapplications,” Applied Thermal Engineering, vol. 23, 2003, pages251-283; and Bo et al., “Tetradecane and hexadecane binary mixtures asphase change materials (PCMs) for cool storage in district coolingsystems,” Energy, vol. 24, 1000, pages 1015-1028; which are eachincorporated by reference.

Methods

FIG. 5 illustrates an optional method of preparation of the metallicsystem components of the apparatus prior to assembly of the apparatus.In order to establish and maintain a substantially reduced gas pressure(e.g. less than or equal to 1×10⁻² torr) within the apparatus, themetallic surfaces of the components of the apparatus may optionally becleaned and prepared to minimize outgassing from surface contaminants onthe metallic surfaces. FIG. 5 depicts, as an example, a flowchart of amethod that may be used in some embodiments to prepare the metallicsystem components of the apparatus as described herein prior to assemblyof the apparatus. See also Y. T. Sasaki, “A survey of vacuum materialcleaning procedures: A subcommittee report of the American VacuumSociety Recommended Practices Committee,” Journal of Vacuum Science &Technology A: Vacuum, Surfaces, and Films, vol. 9, May. 1991, p. 2025,which is incorporated by reference.

FIG. 5 illustrates a flowchart of a method to prepare metallic systemcomponents prior to assembly 500 of an apparatus. Block 510 depictscleaning components with denatured alcohol. This step may reduce grease,oil and similar contaminants on the surfaces of the components. Theflowchart also includes optional block 520, illustrating mechanicallypolishing the components. See, for example, Kato et al., “Achievement ofextreme high vacuum in the order of 10⁻¹⁰ Pa without baking of testchamber,” Journal of Vacuum Science and Technology, vol. A8, no. 3,May/June 1990, pages 2860-2864, which is incorporated by reference. Thisstep may be omitted, for example wherein the components already aresufficiently smooth. See: S. Okamura, “Outgassing measurement of finelypolished stainless steel,” Journal of Vacuum Science & Technology A:Vacuum, Surfaces, and Films, vol. 9, July 1991, p. 2405; M. Suemitsu etal., “Ultrahigh-vacuum compatible minor-polished aluminum-alloy surface:Observation of surface-roughness-correlated outgassing rates,” Journalof Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 10,1992, pp. 570-572; M. Suemitsu et al., “Development of extremely highvacuums with mirror-polished AL-alloy chambers,” Vacuum, vol. 44, nos.5-7, 1993, pages 425-428; H. F. Dylla, “Correlation of outgassing ofstainless steel and aluminum with various surface treatments,” Journalof Vacuum Science & Technology A: Vacuum, Surfaces, and Films, vol. 11,September 1993, p. 2623; Mohri et al., “Surface study of Type 6063aluminum alloys for vacuum chamber materials,” Vacuum, vol. 34, no. 6,1984, pages 643-647; and Y. T. Sasaki, “Reducing SS 304316 hydrogenoutgassing to 2×10 [sup−15] torr 1/cm[sup 2] s,” Journal of VacuumScience & Technology A: Vacuum, Surfaces, and Films, vol. 25, 2007, p.1309, which are all incorporated by reference. If the components aremechanically polished, they may be subsequently cleaned an additionaltime with denatured alcohol (not illustrated in FIG. 5).

Block 530 illustrates washing the components with detergents and water.A detergent washing step may reduce the presence of fine contaminantssuch as hydrocarbon oils and solvents, which may contribute toundesirable outgassing within the finished apparatus. See: R. Elsey,“Outgassing of vacuum materials-II,” Vacuum, vol. 25, 1975, pp. 347-361,which is incorporated by reference. As an example, hand dishwashingdetergent (i.e. Dawn Advanced Power Dish Soap, manufactured by theProcter & Gamble Company) may be used to hand wash the components inwarm tap water and a standard soft sponge. As an additional example, thedetergent Alconox® may be used to clean the components in tap water(available from Alconox Inc., White Plains N.Y.). Optional block 540depicts rinsing the washed components with deionized water (DI water).Optional block 550 illustrates blowing the components dry withdehumidified nitrogen gas, or a comparable inert gas. This step mayreduce non-visible water molecules adhering to the surface of thecomponents. See, for example: A. Berman, “Water vapor in vacuumsystems,” Vacuum, vol. 47, no. 4, 1996, pages 327-332; J.-R. Chen etal., “Outgassing behavior of A6063-EX aluminum alloy and SUS 304stainless steel,” Journal of Vacuum Science and Technology, vol. A5, no.6, November/December 1987, pages 3422-3424; Y. C. Liu et al., “Thermaloutgassing study on aluminum surfaces,” Vacuum, vol. 44, nos. 5-7, 1993,pages 435-437; Chen and Liu, “A comparison of outgassing rate of 304stainless steel and A6063-EX aluminum alloy vacuum chamber after fillingwith water,” Journal of Vacuum Science and Technology, vol. A5, no. 2,March/April 1987, pages 262-264; Ishimaru et al., “Fast pump-downaluminum ultrahigh vacuum system,” Journal of Vacuum Science andTechnology, vol. A10, no. 3, May/June 1992, pages 547-552; Miki et al.,“Characteristics of extremely fast pump-down process in an aluminumultrahigh vacuum system,” Journal of Vacuum Science and Technology, vol.A12, no. 4, July/August 1994, pages 1760-1766; and Chen et al.,“Outgassing behavior on aluminum surfaces: water in vacuum systems,”Journal of Vacuum Science and Technology, vol. A12, no. 4, July/August1994, pages 1750-1754, which are each incorporated by reference. In someembodiments, treatment with different types of gas may be included. See:Tatenuma et al., “Quick acquisition of clean ultrahigh vacuum bychemical process technology,” Journal of Vacuum Science and Technology,vol. All, no. 4, July/August 1993, pages 1719-1724; Tatenuma et al.,“Acquisition of clean ultrahigh vacuum using chemical treatment,”Journal of Vacuum Science and Technology, vol. A16, no. 4, July/August1998, pages 2693-2697; and L. C. Beavis, “Interaction of hydrogen withthe surface of type 304 stainless steel,” Journal of Vacuum Science andTechnology, vol. 10, no. 2, March/April 1973, pages 386-390; which areincorporated by reference. Block 560 depicts baking the components undervacuum conditions. See, for example: H. Ishimaru, “Fast pump-downaluminum ultrahigh vacuum system,” Journal of Vacuum Science &Technology A: Vacuum, Surfaces, and Films, vol. 10, May 1992, p. 547,which is incorporated by reference.

Baking components under vacuum conditions has been demonstrated to beuseful for reducing outgassing from some materials, for example, foraluminum and stainless steel components. See: J. Young, “OutgassingCharacteristics of Stainless Steel and Aluminum with Different SurfaceTreatments,” Journal of Vacuum Science and Technology, 1969; Odaka andUeda, “Dependence of outgassing rate on surface oxide layer thickness intype 304 stainless steel before and after surface oxidation in air,”Vacuum, no. 47, nos. 6-8, 1996, pages 689-692; Odaka et al., “Effect ofbaking temperature and air exposure on the outgassing rate of type 316Lstainless steel,” Journal of Vacuum Science and Technology, vol. A5, no.5, September/October 1987, pages 2902-2906; Zajec and Nemanic, “Hydrogenbulk states in stainless-steel related to hydrogen release kinetics andassociated redistribution phenomena,” Vacuum, vol. 61, 2001, pages447-452; Bernardini et al., “Air bake-out to reduce hydrogen outgassingfrom stainless steel,” Journal of Vacuum Science and Technology, vol.A16, no. 1, January/February 1998, pages 188-193; Nemanic et al.,“Anomalies in kinetics of hydrogen evolution from austenitic stainlesssteel from 300 to 1000° C.,” Journal of Vacuum Science and Technology,vol. A19, no. 1, January/February 2001, pages 215-222; Nemanic andBogataj, “Outgassing of thin wall stainless steel chamber,” Vacuum, vol.50, no. 3-4, 1998, pages 431-437; Cho et al., “Creation of extreme highvacuum with a turbomolecular pumping system: a baking approach,” Journalof Vacuum Science and Technology, vol. A13, no. 4, July/August 1995,pages 2228-2232; and Y. Ishikawa and K. Odaka, “Reduction of outgassingfrom stainless surfaces by surface oxidation,” Vacuum, vol. 41, 1990,pp. 1995-1997; which are incorporated by reference. For example,stainless steel components may be baked for 30 hours at 250 degreesCentigrade in a chamber with a gas pressure of approximately 1×10⁻²torr. As an additional example, aluminum components or compositecomponents may be baked at 150 degrees Centigrade for 60-70 hours in achamber with a gas pressure of approximately 1×10⁻² torr. See also: Chenet al., “An aluminum vacuum chamber for the bending magnet of the SRRCsynchrotron light source,” Vacuum, vol. 41, nos. 7-9, 1990, pages2079-2081; Burns et al., “Outgassing test for non-metallic materialsassociated with sensitive optical surfaces in a space environment,”Materials and Processes Laboaratory, George C. Marshall Space FlightCenter, 1987; and Chen et al., “Thermal outgassing from aluminum alloyvacuum chambers,” Journal of Vacuum Science and Technology, vol. A3, no.6, November/December 1985, pages 2188-2191, which are each incorporatedby reference. In addition or alternately, baking components in thepresence of inert gas has been demonstrated to be useful for reducingoutgassing from some materials. In some embodiments, as an alternate tonear-vacuum gas pressure conditions, the components are baked in thepresence of inert gas, such as nitrogen.

After the components are cleaned and prepared, the components of theapparatus are assembled. A helium leak check may be performed to ensurethat seals and/or junctions are sufficient to maintain reduced gaspressure conditions within the interior of the apparatus. In addition,the apparatus may be purged with dehydrated nitrogen gas during thecheck of the final assembly. See: K. Yamazaki, et al., “High-speedpumping to UHV,” Vacuum, vol. 84, December 2009, pp. 756-759; and Chunet al., “outgassing rate characteristic of a stainless-steel extremehigh vacuum system,” Journal of Vacuum Science and Technology, vol. A14,no. 4, July/August 1996, pages 2636-2640; which are incorporated byreference.

FIG. 6 illustrates a flowchart of a method utilizing an apparatus suchas those described herein (as above). FIG. 6 depicts a method 600,including steps depicted as blocks 610, 620, 630, 640 and 650. Block 610illustrates establishing vacuum within a gas-sealed apparatus includingat least one activation region fabricated from a heat-resistantmaterial, a structural region fabricated from a heat-sensitive material,and a connector between the regions. As used herein, “vacuum” refers tothe gas pressure in substantially evacuated space. As used herein,“vacuum” refers to a low gas pressure relative to the gas pressure inthe environment external to the apparatus. Different levels of vacuummay be suitable in different embodiments. For example, as used herein,“vacuum” refers to substantially evacuated space that may have a gaspressure less than 1×10⁻² torr, less than 5×10⁻³ torr, less than 5×10⁻⁴torr, less than 5×10⁻⁵ torr, less than 5×10⁻⁶ torr or less than 5×10⁻⁷torr. Different gas pressures may be desirable depending on the specificembodiment, including factors such as durability, cost, components,fabrication, structure and expected duration of use. The vacuum may beestablished within an interior of the at least one activation region,within an interior of the at least one structural region, and within aninterior of the connector of the gas-sealed apparatus. The vacuum may beestablished utilizing a vacuum pump operably connected to the gas-sealedapparatus. Suitable vacuum pumps for some embodiments are manufactured,for example, by Pfeiffer Balzers Company, (Pfeiffer Vacuum GmbH,Germany). Suitable vacuum pumps for some embodiments are manufactured,for example, by the Edwards Vacuum Company (US Headquarters TewksburyMass.; Global Headquarters United Kingdom). Vacuum pumps suitable insome embodiments include Pfeiffer Balzers model TSH060 and Edwards modelRV12. See also Ishimaru and Hismatsu, “Turbomolecular pump with anultimate pressure of 10⁻¹² Torr,” Journal of Vacuum Science andTechnology, vol. A12, no. 4, July/August 1994, pages 1695-1698; andJhung et al., “Achievement of extremely high vacuum using a cryopump andconflate aluminum gaskets,” Vacuum, vol. 43, no. 4, 1992, pages 309-311,which are each incorporated by reference.

In some embodiments, heating the apparatus components while establishingthe vacuum may reduce the time required to establish vacuum, for exampleby increasing the rate of evaporation of traces of water on the surfacesof the interior of the apparatus. In order to heat the apparatuscomponents while establishing the vacuum, the apparatus may be placedwithin an oven of suitable size and operating conditions. In addition oralternately, in order to heat the apparatus components whileestablishing the vacuum, the exterior surfaces of the apparatus may bewrapped with heat tape, and the base of the apparatus may be placed on ahot plate. Suitable heat tape for some embodiments includes, forexample, insulated heat tapes and may include fiberglass heavy insulatedheat tapes (e.g. model AIH-0510100 from HTS/Amptek Corporation, StaffordTex.). The gas-sealed apparatus may be heated, for example, intemperature increments to ensure even heating, to allow time to monitorthe apparatus, to allow for maintenance of the low gas pressure withinthe interior, and to ensure that the apparatus does not over-heat. Theapparatus may be heated, as an example, to approximately 130-150 degreesCentigrade in approximately 50 degree increments during establishment ofvacuum within the gas-sealed apparatus. The apparatus may be heated, asan example, to approximately 180-220 degrees Centigrade in approximately20 degree increments during establishment of vacuum within thegas-sealed apparatus. Depending on the embodiment, establishing thevacuum may take several days, even with heating of the apparatuscomponents assisting in a reduction of the time required. For example,establishing the vacuum may take a time on the order of 5-7 days ofcontinual action by the vacuum pump and heating of the apparatuscomponents. Even after suitable cleaning and other preparation,outgassing of volatile materials from the internal surfaces of thegas-sealed apparatus is expected, and will increase the time required toreach a suitably low gas pressure for a given embodiment. For example,heating the gas-sealed apparatus will increase outgassing of materialfrom the internal surfaces of the gas-sealed apparatus. Suitable gaspressure within the interior of the apparatus is established when a gaspressure gauge operably attached to the apparatus displays a reading inthe range appropriate for the embodiment (e.g. a gas pressure less than1×10⁻² torr, less than 5×10⁻³ torr, less than 5×10⁻⁴ torr, less than5×10⁻⁵ torr, less than 5×10⁻⁶ torr or less than 5×10⁻⁷ torr).

The method flowchart depicted in FIG. 6 also includes block 620, showingheating the at least one activation region to an activation temperaturefor an activation time suitable to activate one or more getters withinthe at least one activation region, while maintaining the establishedvacuum within the apparatus. As noted above, the activation temperaturefor a particular embodiment is dependent on the specific gettersincluded in that embodiment. Heating of an activation region includesheating the getters within the activation region to a suitabletemperature. Getters suitable for some embodiments includezirconium-vanadium-iron getters, as described in U.S. Pat. No.4,312,669, ibid., incorporated by reference herein. As noted in U.S.Pat. No. 4,312,669, ibid., incorporated by reference herein, azirconium-vanadium-iron getter material may be activated by heating to atemperature of approximately 700 degrees Centigrade for at least 20seconds and then reducing the temperature to between approximately 400degrees Centigrade and approximately 25 degrees Centigrade. Also asnoted in U.S. Pat. No. 4,312,669, ibid., incorporated by referenceherein, a zirconium-vanadium-iron getter material may be activated byheating to a temperature less than 450 degrees Centigrade, such asapproximately 400 degrees Centigrade, or between approximately 250 andapproximately 350 degrees Centigrade, for a time between 1 and 10minutes while in an environment with a gas pressure of less than 10⁻²torr. In some embodiments, the activation region may be heated to atemperature of approximately 400 degrees Centigrade for at least 45minutes. In some embodiments, the activation region may be heated inintervals of approximately 50 degrees Centigrade.

Heating the at least one activation region to an activation temperaturefor an activation time suitable to activate one or more getters withinthe at least one activation region while maintaining the establishedvacuum within the apparatus may include heating the activation regionindependently from the remainder of the apparatus while the vacuum pumpattached to the apparatus is operating. For example, the activationregion may be heated with a heat source external to the apparatus. Insome embodiments, in order to heat the activation region, the activationregion exclusively to the remainder of the apparatus may be placedwithin an oven of suitable size, shape and properties. In someembodiments, in order to heat the activation region, the exteriorsurfaces of the activation region may be wrapped with heat tape.Suitable heat tape for some embodiments includes, for example, insulatedheat tapes and may include fiberglass heavy insulated heat tapes (e.g.model AIH-0510100 from HTS/Amptek Corporation, Stafford Tex.). Heatingthe activation region may include heating with a heat source in directthermal contact with the activation region and not in direct thermalcontact with the structural region and the connector of the gas-sealedapparatus. For example, if heat tape is used, a specific section of heattape may be wrapped around the outer surface of the activation regionand set to a temperature higher than any temperature setting for theremainder of the apparatus.

The method flowchart depicted in FIG. 6 also includes block 630,illustrating allowing the at least one activation region and the gettersto cool to a temperature compatible with structural stability of theheat-sensitive material. The activation region may be cooled throughradiative heat loss. For example, in embodiments where heat tape is usedto heat the external surface of the activation region, the heat tape maybe removed and the activation region allowed to cool by heat radiationinto the external environment. In some embodiments, the activationregion may be allowed to cool to a specific temperature, or temperaturerange, such as approximately 100 degrees Centigrade, approximately 150degrees Centigrade, approximately 200 degrees Centigrade, approximately250 degrees Centigrade, approximately 300 degrees Centigrade, orapproximately 350 degrees Centigrade.

As shown in FIG. 6, the method flowchart also includes block 640,depicting transferring the cooled one or more getters from the cooled atleast one activation region to the structural region through theconnector, while maintaining the established vacuum within thegas-sealed apparatus. For example, the cooled getters may be transferredthrough the gas-sealed apparatus by gravitational transfer, such asthrough reorienting the relative positions of the activation region andthe structural region and allowing the getters to move through gravitythrough the apparatus (see FIGS. 1-4 and associated text, above). Forexample, the cooled getters may be transferred through the apparatusthrough a mechanical transfer, such as with an internal trowel, scoop,ladle, or fork configured to transfer the cooled getters within thegas-sealed apparatus.

The flowchart depicted in FIG. 6 also includes block 650, illustratingseparating the connector between the regions while maintaining thevacuum within the structural region including the cooled one or moregetters. For example, the connector may be separated at a regionadjacent to the surface of the outer wall of the structural region bycrimping the connector sufficiently to establish a gas-tight seal, andseparating the connector into two parts at the crimped region. Anultrasonic welder may be utilized to separate the connector between theregions while maintaining the vacuum within the structural regionincluding the cooled one or more getters. A specialized crimping devicemay be used to separate the connector between the regions whilemaintaining the vacuum within the structural region including the cooledone or more getters.

FIG. 7 illustrates additional aspects of the method illustrated in theflowchart of FIG. 6. FIG. 7 shows block 610, which illustratesestablishing vacuum within a gas-sealed apparatus including at least oneactivation region fabricated from a heat-resistant material, astructural region fabricated from a heat-sensitive material, and aconnector between the regions. Optional blocks 700, 710 and 720illustrate optional aspects of the method. Block 700 illustratesestablishing vacuum within an interior of the at least one activationregion, within an interior of the at least one structural region, andwithin an interior of the connector of the gas-sealed apparatus. Forexample, vacuum may be established using a vacuum pump operably attachedto the apparatus and the methods described herein. In some embodiments,additionally heating the apparatus may decrease the time required toestablish vacuum within the gas-sealed apparatus including at least oneactivation region fabricated from a heat-resistant material, astructural region fabricated from a heat-sensitive material, and aconnector between the regions. Block 710 depicts utilizing a vacuum pumpoperably connected to the gas-sealed apparatus. For example, someembodiments may utilize a rotary vane style vacuum pump. Suitable vacuumpumps for some embodiments are manufactured, for example, by PfeifferBalzers Company, (Pfeiffer Vacuum GmbH, Germany). Suitable vacuum pumpsfor some embodiments are manufactured, for example, by the EdwardsVacuum Company (US Headquarters Tewksbury Mass.; Global HeadquartersUnited Kingdom). Vacuum pumps suitable in some embodiments includePfeiffer Balzers model TSH060 and Edwards model RV12. FIG. 7 includesblock 720, depicting establishing gas pressure less than or equal to1×10⁻² torr within the gas-sealed apparatus including at least oneactivation region fabricated from a heat-resistant material, astructural region fabricated from a heat-sensitive material, and aconnector between the regions. In some embodiments, the gas pressureestablished within the gas-sealed apparatus including at least oneactivation region fabricated from a heat-resistant material, astructural region fabricated from a heat-sensitive material, and aconnector between the regions may be less than 5×10⁻³ torr, less than5×10⁻⁴ torr, less than 5×10⁻⁵ torr, less than 5×10⁻⁶ torr or less than5×10⁻⁷ torr.

FIG. 8 illustrates additional aspects of the method flowchart depictedin FIG. 7. Flowchart block 620 depicts heating the at least oneactivation region to an activation temperature for an activation timesuitable to activate one or more getters within the at least oneactivation region, while maintaining the established vacuum within theapparatus. Flowchart block 620 may include one or more of optionalblocks 800 and 810. Block 800 depicts heating the activation region to atemperature of approximately 400 degrees Centigrade for at least 45minutes. The activation region should be heated to a temperature and fora duration sufficient to activate the particular type of getters withinthe activation region given the conditions of a particular embodiment,such as the size, shape and position of the getters as well as the gaspressure within the activation region. As described herein, theactivation temperature and activation conditions (e.g. time and gaspressure) of the particular type of getters used in a particularembodiment is the basis for determining the heating temperature and timeof the activation region. Block 810 illustrates heating the activationregion with a heat source external to the apparatus. For example,exclusively of the remainder of the apparatus the activation region maybe placed within an oven of suitable size, shape and operatingparameters. For example, the outer surface of the activation region maybe heated with a heat tape wrapped around the activation region of theapparatus. Suitable heat tape for some embodiments includes, forexample, insulated heat tapes and may include fiberglass heavy insulatedheat tapes (e.g. model AIH-0510100 from HTS/Amptek Corporation, StaffordTex.). Heating the activation region may include heating with a heatsource in direct thermal contact with the activation region and not indirect thermal contact with the structural region and the connector ofthe gas-sealed apparatus.

FIG. 9 illustrates aspects of the method flowchart as illustrated inFIG. 6. Flowchart block 620 depicts heating the at least one activationregion to an activation temperature for an activation time suitable toactivate one or more getters within the at least one activation region,while maintaining the established vacuum within the apparatus. Flowchartblock 620 may include one or more of optional blocks 900 and 910. Block900 depicts heating the activation region with a heat source in directthermal contact with the activation region and not in direct thermalcontact with the structural region and the connector of the gas-sealedapparatus. For example, heat tape may be wrapped around the exteriorsurface of the activation region and not other regions of the apparatus,and the heat tape specifically controlled independently of any othercontrols. Block 910 illustrates heating the at least one activationregion in intervals of approximately 50 degrees Centigrade. For example,if the at least one activation region is initially at a temperature ofapproximately 25 degrees Centigrade, the at least one activation regionmay be heated to approximately 75 degrees Centigrade, then 125 degreesCentigrade, then 175 degrees Centigrade, and so on until the finaldesired activation temperature is reached.

FIG. 10 depicts aspects of the method flowchart illustrated in FIG. 6.Block 630 shows allowing the at least one activation region and thegetters to cool to a temperature compatible with structural stability ofthe heat-sensitive material. Flowchart block 630 may include one or moreof optional blocks 1000 and 1010. Block 1000 illustrates allowing the atleast one activation region to cool to an ambient temperature throughradiative heat loss. For example, any heat tape may be turned off,allowed to cool, and then removed from the exterior surface of anactivation region. The activation region then is allowed to cool toeither a predetermined temperature or an ambient temperature throughradiative heat loss. Block 1010 depicts allowing the at least oneactivation region to cool to approximately 250 degrees Centigrade. Forexample, approximately 250 degrees Centigrade may be a temperaturecompatible with structural stability of a heat-sensitive material suchas aluminum.

FIG. 11 shows aspects of the method flowchart illustrated in FIG. 6.Block 640 shows transferring the cooled one or more getters from thecooled at least one activation region to the structural region throughthe connector, while maintaining the established vacuum within theapparatus. Block 640 may include one or more of optional blocks 1100 and1110. Block 1100 depicts bending the connector to allow the cooled oneor more getters to move from the cooled at least one activation regionto the at least one structural region through the connector. Forexample, the method may include bending a flexible region of theconnector to place the activation region in a position substantiallyabove the structural region, allowing the getters to fall through theforce of gravity from the one activation region to the structural regionthrough the connector. The vacuum pump may be operational during thegetter transfer to maintain the established vacuum within the apparatus.Block 1110 illustrates bending the connector to alter the relativepositioning of the cooled at least one activation region to the at leastone structural region in relation to the connector. For example, themethod may include bending the connector to alter the relative positionof the at least one activation region relative to the structural region.

FIG. 12 depicts aspects of the method flowchart illustrated in FIG. 6.Block 640 shows transferring the cooled one or more getters from thecooled at least one activation region to the structural region throughthe connector, while maintaining the established vacuum within theapparatus. Block 640 may include optional block 1200. Block 1200 showstransferring the cooled one or more getters into a gas-sealed gapbetween an inner wall and an outer wall of the structural region. Forexample, the activation region may be positioned so that the connectoris in a substantially linear configuration, and oriented so that theopening of the activation region attached to the connector isapproximately directly above an opening into the gas-sealed gap that isoperably attached to the connector. Block 650 shows separating theconnector between the regions while maintaining the vacuum within thestructural region including the cooled one or more getters. For example,the connector may be crimped and separated at a region adjacent to theouter surface of the structural region. Block 650 may include optionalblock 1210. Block 1210 depicts sealing the connector at a positionadjacent to the structural region. For example, as illustrated in FIGS.1-4, the connector may include a region configured for sealing anddetachment of the structural region from the activation region in alocation adjacent to the structural region. The region configured forsealing and detachment of the structural region from the activationregion need not be directly next to the exterior surface of thestructural region; as shown in FIGS. 1-4, there may be a section of theconnector between the exterior surface of the structural region and theposition where the connector is sealed and detached.

FIG. 13 shows aspects of the method flowchart illustrated in FIG. 6.Block 650 shows separating the connector between the regions whilemaintaining the vacuum within the structural region including the cooledone or more getters. For example, the connector may be welded togetherand then disconnected using an ultrasonic welding device. Block 650 mayinclude optional block 1300. Block 1300 depicts crimping the connector;and breaking the connector at the crimp location. For example, anultrasonic welder may be used to weld to opposite faces of the connectortogether, and then to break the connector at the weld joint. Forexample, a crimping device specialized to crimp the connectorsufficiently to form a gas-impermeable seal may be used, and theconnector then broken at the seal location. As shown in FIG. 13, themethod flowchart may also include optional block 1310. Block 1310depicts adding sealing material to a surface of the separated connectoradjacent to the structural region including the cooled one or moregetters. Sealing material, such as epoxy material, may be added to thesurface of the separated connector, such as over the crimp or weld site.See also FIG. 4 and associated text.

FIG. 14 depicts aspects of the method flowchart shown in FIG. 6. FIG. 14illustrates that the flowchart may include one or more of optionalblocks 1400 and 1410. Block 1400 may include block 1410. Block 1400shows heating the structural region to a preset temperature for apredetermined time after establishing vacuum within the structuralregion and before heating the activation region. For example, thestructural region may be heated to approximately 150 degrees tofacilitate establishment of a durable vacuum within the apparatus. Forexample, the structural region may be heated with heat tape placed onthe external surface of the structural region. For example, thestructural region may be placed on a heat plate. Block 1410 depictsheating the structural region to the preset temperature by intervals ofapproximately 50 degrees Centigrade. For example, if starting at anambient temperature of approximately 25 degrees Centigrade, thestructural region may be heated to approximately 75 degrees Centigrade,then to approximately 125 degrees Centigrade, then to approximately 175degrees Centigrade, then to approximately 225 degrees Centigrade, and soon until the desired temperature is reached. The heating series may beheld at any or all of the series of temperatures for a given timeperiod, for example for 10 minutes, 1 hour, 5 hours, or 1 day.

FIG. 15 illustrates aspects of the method flowchart shown in FIG. 6.FIG. 15 illustrates that the flowchart may include optional block 1500.Block 1500 depicts heating the structural region to a preset temperatureprior to transferring the cooled one or more getters; and maintainingthe preset temperature while separating the connector. For example, thestructural region may be placed on a hot plate heated to a presettemperature before the transfer of the cooled one or more getters, andthe structural region maintained on the hot plate set to a constanttemperature during transfer of the getters. For example, the structuralregion may be wrapped with heat tape and heated to a preset temperatureprior to the transfer of the getters, and the temperature maintainedduring the transfer. For example, the structural region may be heated toa predetermined temperature between approximately 125 degrees Centigradeand approximately 175 degrees Centigrade, and this temperaturemaintained during the getter transfer. For example, the structuralregion may be heated to a predetermined temperature betweenapproximately 175 degrees Centigrade and approximately 225 degreesCentigrade, and this temperature maintained during the getter transfer.For example, the structural region may be heated to a predeterminedtemperature between approximately 200 degrees Centigrade andapproximately 250 degrees Centigrade, and this temperature maintainedduring the getter transfer.

FIG. 16 illustrates a flowchart of a method. Block 1600 of the flowchartillustrates that the method is of establishing and maintaining vacuumwithin a storage device. Block 1600 includes blocks 1610, 1620, 1630,1640, 1650, 1660, 1670, 1680 and 1690. Block 1610 illustrates assemblingthe components of a storage device, including an outer wall and an innerwall substantially defining a gas-sealed gap. Block 1620 depictsattaching the storage device to an apparatus, the apparatus including agetter activation region containing one or more getters, a vacuum pump,and a connector operably connecting the storage device to the apparatus.Block 1630 shows activating the vacuum pump to establish gas pressurebelow atmospheric pressure within the gas-sealed gap of the storagedevice. Block 1640 illustrates heating the storage device to apredetermined temperature for a predetermined length of time. Block 1650shows heating the getter activation region and the one or more gettersto an activation temperature for an activation time suitable to activateone or more getters within the at least one activation region, whilemaintaining the established gas pressure below atmospheric pressurewithin the gas-sealed gap of the storage device. Block 1660 illustratesallowing the getter activation region and the one or more getters tocool to a predetermined temperature. Block 1670 shows flexing theconnector to move the storage device and the getter activation regioninto a relative position wherein the getter activation region is abovethe storage device and the connector is substantially linear. Block 1680depicts allowing the getters to fall along the connector interior intothe gas-sealed gap in the storage device, while maintaining theestablished gas pressure below atmospheric pressure within thegas-sealed gap of the storage device. Block 1690 shows separating theconnector at a location adjacent to the storage device while maintainingthe established gas pressure below atmospheric pressure within thegas-sealed gap of the storage device.

Block 1620 depicts attaching the storage device to an apparatus, theapparatus including a getter activation region containing one or moregetters, a vacuum pump, and a connector operably connecting the storagedevice to the apparatus. For example, the assembled device may beattached to an apparatus with a substantially gas-impermeable junctionto form an apparatus such as illustrated in FIGS. 1-4. As shown in FIGS.1-4, the interior of the apparatus includes a gas-sealed space withinthe getter activation region, the connector and the gas-sealed gap ofthe storage device. The gas-sealed gasp within a storage device may beconnected to an apparatus through a conduit, for example with one ormore ducts as illustrated as 175 in FIG. 23.

FIG. 17 illustrates aspects of the flowchart depicted in FIG. 16. FIG.17 illustrates that block 1610 may include optional block 1700. Block1610 illustrates assembling the components of a storage device,including an outer wall and an inner wall substantially defining agas-sealed gap. For example, the components of a storage device may beassembled into a device as illustrated in FIGS. 1-4 and in FIG. 23. Asshown in FIG. 17, block 1610 may include optional block 1700. Block 1700depicts assembling the components of the storage device to form agas-sealed gap within the storage device. For example, there may bejoints, welds or seals included in the assembled components to create agas-impermeable seal around the perimeter of the gas-sealed gap withinthe storage device.

FIG. 17 shows further aspects of the flowchart depicted in FIG. 16. FIG.17 illustrates that block 1630 may include optional block 1710. Block1630 depicts activating the vacuum pump to establish gas pressure belowatmospheric pressure within the gas-sealed gap of the storage device.For example, one or more vacuum pumps may be utilized to establishsubstantially evacuated space within the gas-sealed gap of the storagedevice. For example, one or more vacuum pumps may be utilized toestablish an extremely low gas pressure within the gas-sealed gap of thestorage device. Block 1710 illustrates establishing a gas pressure ofless than or equal to 1×10⁻² ton. For example, one or more vacuum pumpsmay be utilized to establish a gas pressure less than 5×10⁻³ torr, lessthan 5×10⁻⁴ torr, less than 5×10⁻⁵ torr, less than 5×10⁻⁶ torr or lessthan 5×10⁻⁷ torr within the gas-sealed gap of the storage device.

FIG. 18 illustrates additional aspects of the flowchart shown in FIG.16. Block 1640 illustrates heating the storage device to a predeterminedtemperature for a predetermined length of time. For example, the storagedevice may be heated with an external heat source to a predeterminedtemperature for a length of time estimated to be required to evaporateany surface contaminants on the interior surface of the gas-sealed gapof the storage device. For example, the storage device may be heatedwith an external heat source to a predetermined temperature for a lengthof time estimated to be required to dehydrate the interior surface ofthe gas-sealed gap of the storage device. The heating temperature andtime will depend on the specific embodiment, for example the type ofmaterial used to fabricate the storage device, the prior surfacetreatment of the material (for example as described in relation to FIG.5, text above), and the desired final gas pressure within the gas-sealedgap of the storage device. FIG. 18 illustrates that block 1640 mayinclude one or more of optional blocks 1800 and 1810. Block 1800illustrates heating the storage device in increments of approximately 50degrees Centigrade. For example, in an embodiment where heat tapewrapped around the exterior of the storage device is implemented to heatthe storage device, the controller for the heat tape may be set to warmthe heat tape in approximately 50 degree Centigrade increments. Warmingthe storage device in increments may be desirable, for example, to avoidoverheating, or to ensure that the storage device is heated evenlythroughout the surface, or to confirm that the junctions between thestorage device and the connector are retaining a gas seal during theprocess. Warming the storage device in increments may be desirable, forexample, to allow for time to check the gas pressure internal to theapparatus during the process. Block 1810 illustrates heating the storagedevice to between approximately 130 degrees Centigrade and approximately150 degrees Centigrade for at least 100 hours. The specific time andtemperature will depend on the embodiment, and the time required toreduce the internal gas pressure of the apparatus to a target gaspressure. For example, the specific time and temperature will depend onfactors including the material used to fabricate the storage device, anypretreatment of the components, the size and shape of the gas-sealedgap, the size and shape of the interior of the apparatus, and thepumping capacity of the vacuum pump in a given embodiment. In someembodiments, the storage device may be heated to between approximately150 degrees Centigrade and approximately 200 degrees Centigrade. In someembodiments, the storage device may be heated for approximately 75hours. In some embodiments, the storage device may be heated forapproximately 100 hours, or approximately 125 hours.

FIG. 19 shows additional aspects of the flowchart shown in FIG. 16.Block 1650 illustrates heating the getter activation region and the oneor more getters to an activation temperature for an activation timesuitable to activate one or more getters within the at least oneactivation region, while maintaining the established gas pressure belowatmospheric pressure within the gas-sealed gap of the storage device. Asdiscussed above, the activation temperature and time required in aspecific embodiment depends on the getters used. For example, as notedin U.S. Pat. No. 4,312,669, ibid., incorporated by reference herein, azirconium-vanadium-iron getter material may be activated by heating to atemperature less than 450 degrees Centigrade, such as approximately 400degrees Centigrade, or between approximately 250 and approximately 350degrees Centigrade, for a time between 1 and 10 minutes while in anenvironment with a gas pressure of less than 10⁻² torr. Also relevant isthe material used in the fabrication of the activation region includingthe getters, clearly a user of the apparatus and method would not heatthe getter activation region to a temperature predicted to compromisethe structural integrity of the activation region. For example, a userof the apparatus and method would not heat the getter activation regionto a temperature wherein the getter activation region could not maintainits shape and structure in response to the internal force of the low gaspressure. For example, a user of the apparatus and method would not heatthe getter activation region to a temperature wherein the getteractivation region would be predicted to melt, implode or deform based onthe material and fabrication of the structure.

FIG. 19 illustrates that the flowchart of FIG. 16 may also include oneor more of optional blocks 1900 and 1910 within block 1650. Block 1900depicts heating the activation region to a temperature of approximately400 degrees Centigrade for at least 45 minutes. For example, inembodiments employing a zirconium-vanadium-iron getter material, thegetter material may be activated at approximately 400 degrees Centigradefor a duration of at least 45 minutes (see U.S. Pat. No. 4,312,669,ibid., incorporated by reference herein). Block 1910 illustrates heatingthe getter activation region with a heat source external to the getteractivation region. For example, the getter activation region may bewrapped with heat tape on the external surface of the getter activationregion as a heat source. For example, the getter activation region maybe placed in direct contact with a hot plate or similar heating surfaceas a heat source.

FIG. 20 depicts aspects of the method flowchart shown in FIG. 16. Theflowchart shown in FIG. 20 depicts the method of establishing andmaintaining vacuum within a storage device 1600 as illustrated in FIG.16, as well as flowchart blocks 1610, 1620, 1630, 1640, 1650, 1660,1670, 1680, 190 and optional blocks 2000 and 2010. The flowchart shownin FIG. 20 includes block 1660, showing allowing the getter activationregion and the one or more getters to cool to a predeterminedtemperature. For example, after heating (as illustrated in block 1650),the getter activation region and the one or more getters may be cooledto a temperature compatible with further steps of the method. Forexample, after heating (as illustrated in block 1650), the getteractivation region and the one or more getters may be cooled to atemperature compatible with allowing the getters to fall along theconnector interior into the gap in the storage device (as shown in block1680). For example, the getter activation region and the getters may becooled to a temperature compatible with the structural integrity of theconnector). For example, the getter activation region and the gettersmay be cooled to a temperature compatible with the structural integrityof the storage device. The predetermined temperature(s) will depend onfactors including the material used to fabricate the regions of theapparatus, as well as safe and desirable handling temperatures for theapparatus in a given embodiment. Temperatures of the activation regionmay be determined through means suitable to a given embodiment, such asestimates based on the external surface conditions of the activationregion. In some embodiments, there may be an embedded temperature sensorwithin the activation region.

FIG. 20 illustrates that the flowchart depicted in FIG. 16 may includeoptional block 2000 within block 1660. Block 2000 shows allowing thegetter activation region to cool to approximately 250 degrees Centigradethrough radiative heat loss. For example, in embodiments using heat tapeon the exterior surface of the activation region to heat the activationregion, the heat tape may be entirely or partially removed and theactivation region allowed to cool through radiative heat loss from theexternal surface. For example, in embodiments wherein the activationregion is placed in direct physical contact with a surface of a heatsource (e.g. a hot plate), the activation region may be removed from theheat source and allowed to cool. The temperature of the surface of theactivation region may be used as an approximation for the temperature ofthe entire activation region and its contents (e.g. the one or moregetters). In some embodiments, there may be a temperature sensor withinthe interior of the activation region and the reading of thattemperature sensor may be utilized in the method.

As shown in FIGS. 16 and 20, the flowchart includes block 1670, whichdepicts flexing the connector to move the storage device and the getteractivation region into a relative position wherein the getter activationregion is above the storage device and the connector is substantiallylinear. For example, as illustrated in FIGS. 1-4, the shape of theconnector may be altered to allow the getter activation region to bemoved to a position substantially above an opening in the gap in thestorage device and for the connector to be substantially straight. Theconnector may be flexed into a position that allows for the activatedgetters to fall from an opening in the getter activation region throughthe interior of the connector and into the gap in the storage device. Asshown in FIG. 20, block 1670 may include optional block 2010. Block 2010shows flexing the connector to move the storage device and the getteractivation region into a relative position wherein the getter activationregion is above the storage device and the connector is substantiallylinear by flexing a region of the connector adjacent to the getteractivation region. For example, as illustrated in FIGS. 1-4 anddescribed in the associated text (see above), the connector may includea flexible region, such as a region in a corrugated or bellows-typeconfiguration, adjacent to the activation region. The flexible portionof the connector adjacent to the activation region may be flexed to movethe storage device and the getter activation region into a relativeposition wherein the getter activation region is substantially above thestorage device.

FIG. 21 illustrates aspects of the flowchart depicted in FIG. 16. FIGS.16 and 21 include block 1690, depicting separating the connector at alocation adjacent to the storage device while maintaining theestablished gas pressure below atmospheric pressure within thegas-sealed gap of the storage device. For example, the connector may besealed at a location adjacent to the storage device and then twosections of the connector separated either at the seal site or adjacentto the seal site in a manner to maintain the established gas pressurebelow atmospheric pressure within the gas-sealed gap of the storagedevice. FIG. 21 shows that block 1690 of the flowchart may include oneor more of optional blocks 2100 and 2110. Block 2100 depicts physicallycrimping the connector; and breaking the connector at the crimplocation. For example, the connector may be flattened at a locationadjacent to the storage device by physically pressing together the sidesof the connector with a crimping device sufficient to create agas-sealed region in the connector at the crimp site. After theconnector is sufficiently crimped to create a gas-tight seal in theconnector, the connector may be physically broken into two pieces at thecrimp location. If desired, an additional sealing or stabilizationmaterial (e.g. epoxy) may be added to the external surface of theconnector to stabilize the sealed surface (see also item 400 in FIG. 4).Block 2110 depicts separating the connector at a location adjacent tothe storage device while maintaining the established gas pressureutilizing an ultrasonic welding device.

FIG. 22 depicts further aspects of the flowchart as shown in FIG. 16.FIG. 22 shows that block 1600, the method of establishing andmaintaining vacuum within a storage device, may include one or more ofoptional blocks 2200, 2210, 2220 and 2230. Block 2200 illustratesheating the storage device to a predetermined temperature for apredetermined time after establishing gas pressure below atmosphericpressure within the gap of the storage device. For example, it may bedesirable in some embodiments to dehydrate the interior surfaces of thegas-sealed gap in the storage device (e.g. item 190 in FIG. 1) throughheating prior to the connector being sealed. For example, it may bedesirable in some embodiments to heat the storage device to atemperature similar to the temperature of the getters when they areplaced within the gas-sealed gap to ensure even heating and associatedexpansion of the storage device prior to addition of the heated getters.Block 2210 illustrates monitoring gas pressure within the gas-sealed gapof the storage device. For example, it may be desirable in someembodiments to attach a gas pressure gauge to the storage device. FIG.23, for example, illustrates two ducts 175 attached to the outer wall150 of the structural region 180 including a storage device. A gaspressure gauge could be attached to one of the ducts 175 if desired in aspecific embodiment. Block 2220 shows monitoring gas pressure within theconnector. A gas pressure gauge, for example, may be operably attachedto the connector through a duct or a similar structure and used tomonitor gas pressure within the connector during one or more steps ofthe method. Block 2230 shows adding sealing material to the surface ofthe separated connector adjacent to the storage device. For example, anepoxy compound may be added to the surface of the separated connectoradjacent to the storage device (see also item 400 in FIG. 4).

One skilled in the art will recognize that the herein describedcomponents (e.g., operations), devices, objects, and the discussionaccompanying them are used as examples for the sake of conceptualclarity and that various configuration modifications are contemplated.Consequently, as used herein, the specific exemplars set forth and theaccompanying discussion are intended to be representative of their moregeneral classes. In general, use of any specific exemplar is intended tobe representative of its class, and the non-inclusion of specificcomponents (e.g., operations), devices, and objects should not be takenlimiting.

The herein described subject matter sometimes illustrates differentcomponents contained within, or connected with, different othercomponents. It is to be understood that such depicted architectures aremerely exemplary, and that in fact many other architectures may beimplemented which achieve the same functionality. In a conceptual sense,any arrangement of components to achieve the same functionality iseffectively “associated” such that the desired functionality isachieved. Hence, any two components herein combined to achieve aparticular functionality can be seen as “associated with” each othersuch that the desired functionality is achieved, irrespective ofarchitectures or intermedial components. Likewise, any two components soassociated can also be viewed as being “operably connected”, or“operably coupled,” to each other to achieve the desired functionality,and any two components capable of being so associated can also be viewedas being “operably couplable,” to each other to achieve the desiredfunctionality. Specific examples of operably couplable include but arenot limited to physically mateable and/or physically interactingcomponents, and/or wirelessly interactable, and/or wirelesslyinteracting components, and/or logically interacting, and/or logicallyinteractable components.

While particular aspects of the present subject matter described hereinhave been shown and described, it will be apparent to those skilled inthe art that, based upon the teachings herein, changes and modificationsmay be made without departing from the subject matter described hereinand its broader aspects and, therefore, the appended claims are toencompass within their scope all such changes and modifications as arewithin the true spirit and scope of the subject matter described herein.It will be understood by those within the art that, in general, termsused herein, and especially in the appended claims (e.g., bodies of theappended claims) are generally intended as “open” terms (e.g., the term“including” should be interpreted as “including but not limited to,” theterm “having” should be interpreted as “having at least,” the term“includes” should be interpreted as “includes but is not limited to,”etc.). It will be further understood by those within the art that if aspecific number of an introduced claim recitation is intended, such anintent will be explicitly recited in the claim, and in the absence ofsuch recitation no such intent is present. For example, as an aid tounderstanding, the following appended claims may contain usage of theintroductory phrases “at least one” and “one or more” to introduce claimrecitations. However, the use of such phrases should not be construed toimply that the introduction of a claim recitation by the indefinitearticles “a” or “an” limits any particular claim containing suchintroduced claim recitation to claims containing only one suchrecitation, even when the same claim includes the introductory phrases“one or more” or “at least one” and indefinite articles such as “a” or“an” (e.g., “a” and/or “an” should typically be interpreted to mean “atleast one” or “one or more”); the same holds true for the use ofdefinite articles used to introduce claim recitations. In addition, evenif a specific number of an introduced claim recitation is explicitlyrecited, those skilled in the art will recognize that such recitationshould typically be interpreted to mean at least the recited number(e.g., the bare recitation of “two recitations,” without othermodifiers, typically means at least two recitations, or two or morerecitations). Furthermore, in those instances where a conventionanalogous to “at least one of A, B, and C, etc.” is used, in generalsuch a construction is intended in the sense one having skill in the artwould understand the convention (e.g., “a system having at least one ofA, B, and C” would include but not be limited to systems that have Aalone, B alone, C alone, A and B together, A and C together, B and Ctogether, and/or A, B, and C together, etc.). In those instances where aconvention analogous to “at least one of A, B, or C, etc.” is used, ingeneral such a construction is intended in the sense one having skill inthe art would understand the convention (e.g., “a system having at leastone of A, B, or C” would include but not be limited to systems that haveA alone, B alone, C alone, A and B together, A and C together, B and Ctogether, and/or A, B, and C together, etc.). It will be furtherunderstood by those within the art that typically a disjunctive wordand/or phrase presenting two or more alternative terms, whether in thedescription, claims, or drawings, should be understood to contemplatethe possibilities of including one of the terms, either of the terms, orboth terms unless context dictates otherwise. For example, the phrase “Aor B” will be typically understood to include the possibilities of “A”or “B” or “A and B.”

With respect to the appended claims, those skilled in the art willappreciate that recited operations therein may generally be performed inany order. Also, although various operational flows are presented in asequence(s), it should be understood that the various operations may beperformed in other orders than those which are illustrated, or may beperformed concurrently. Examples of such alternate orderings may includeoverlapping, interleaved, interrupted, reordered, incremental,preparatory, supplemental, simultaneous, reverse, or other variantorderings, unless context dictates otherwise. Furthermore, terms like“responsive to,” “related to,” or other past-tense adjectives aregenerally not intended to exclude such variants, unless context dictatesotherwise.

With respect to the use of substantially any plural and/or singularterms herein, those having skill in the art can translate from theplural to the singular and/or from the singular to the plural as isappropriate to the context and/or application. The varioussingular/plural permutations are not expressly set forth herein for sakeof clarity.

All of the above U.S. patents, U.S. patent application publications,U.S. patent applications, foreign patents, foreign patent applicationsand non-patent publications referred to in this specification and/orlisted in any Application Data Sheet, are incorporated herein byreference, to the extent not inconsistent herewith.

While various aspects and embodiments have been disclosed herein, otheraspects and embodiments will be apparent to those skilled in the art.The various aspects and embodiments disclosed herein are for purposes ofillustration and are not intended to be limiting, with the true scopeand spirit being indicated by the following claims.

1. An apparatus comprising: a structural region fabricated from aheat-sensitive material, the structural region including an outer walland an inner wall with a gas-sealed gap between the outer wall and theinner wall; an activation region fabricated from a heat-resistantmaterial, the activation region including one or more getters; aconnector attached to the structural region and to the activationregion, the connector including a flexible region and a regionconfigured for sealing and detachment of the structural region from theactivation region; and a vacuum pump operably attached to the connector.2. The apparatus of claim 1, wherein the structural region comprises: astorage device.
 3. (canceled)
 4. The apparatus of claim 1, wherein thestructural region comprises: a thermally-insulated device.
 5. Theapparatus of claim 1, wherein the structural region comprises: a deviceconfigured for detachment from a remainder of the apparatus. 6.(canceled)
 7. The apparatus of claim 1, wherein the heat-sensitivematerial comprises: aluminum. 8.-11. (canceled)
 12. The apparatus ofclaim 1, wherein the gas-sealed gap comprises: multilayer insulationmaterial.
 13. The apparatus of claim 1, wherein the gas-sealed gapcomprises: gas at a pressure less than or equal to 1×10⁻² torr.
 14. Theapparatus of claim 1, wherein the gas-sealed gap is open to an interiorof the connector.
 15. The apparatus of claim 1, wherein theheat-resistant material comprises: stainless steel.
 16. (canceled) 17.The apparatus of claim 1, wherein the activation region comprises: agas-sealed interior, wherein the one or more getters are enclosed withinthe gas-sealed interior.
 18. The apparatus of claim 17, wherein thegas-sealed interior is open to an interior of the connector.
 19. Theapparatus of claim 1, wherein the one or more getters comprise:non-evaporatable getter material. 20.-21. (canceled)
 22. The apparatusof claim 1, wherein the connector comprises: stainless steel.
 23. Theapparatus of claim 1, wherein the connector comprises: a valveconfigured to inhibit the flow of gas within the connector. 24.(canceled)
 25. The apparatus of claim 1, wherein the flexible region ofthe connector has a bellows configuration.
 26. The apparatus of claim 1,wherein the vacuum pump is sufficient to evacuate an interior of thestructural region, the activation region and the connector to a gaspressure less than or equal to 1×10⁻² torr.
 27. (canceled)
 28. Theapparatus of claim 1, comprising: a gas-sealed, connected space interiorto each of the structural region, the activation region and theconnector.
 29. (canceled)
 30. The apparatus of claim 1, furthercomprising: a pressure gauge operably connected to the connector. 31.The apparatus of claim 1, further comprising: one or more seals betweenthe structural region, the activation region and the connector, theseals sufficient to maintain a vacuum within the structural region, theactivation region and the connector.
 32. A method comprising:establishing vacuum within a gas-sealed apparatus including at least oneactivation region fabricated from a heat-resistant material, astructural region fabricated from a heat-sensitive material, and aconnector between the regions; heating the at least one activationregion to an activation temperature for an activation time suitable toactivate one or more getters within the at least one activation region,while maintaining the established vacuum within the gas-sealedapparatus; allowing the at least one activation region and the one ormore getters to cool to a temperature compatible with structuralstability of the heat-sensitive material; transferring the cooled one ormore getters from the cooled at least one activation region to thestructural region through the connector, while maintaining theestablished vacuum within the gas-sealed apparatus; and separating theconnector between the regions while maintaining the established vacuumwithin the structural region including the cooled one or more getters.33. The method of claim 32, wherein the establishing vacuum comprises:establishing vacuum within an interior of the at least one activationregion, within an interior of the structural region, and within aninterior of the connector of the gas-sealed apparatus.
 34. (canceled)35. The method of claim 32, wherein the establishing vacuum comprises:establishing gas pressure less than or equal to 1×10⁻² torr. 36.(canceled)
 37. The method of claim 32, wherein the heating the at leastone activation region to an activation temperature for an activationtime suitable to activate one or more getters within the at least oneactivation region comprises: heating the at least one activation regionwith a heat source external to the apparatus.
 38. The method of claim32, wherein the heating the at least one activation region to anactivation temperature for an activation time suitable to activate oneor more getters within the at least one activation region comprises:heating the at least one activation region with a heat source in directthermal contact with the at least one activation region and not indirect thermal contact with the structural region and the connector ofthe gas-sealed apparatus.
 39. (canceled)
 40. The method of claim 32,wherein the allowing the at least one activation region and the one ormore getters to cool to a temperature compatible with structuralstability of the heat-sensitive material comprises: allowing the atleast one activation region to cool to an ambient temperature throughradiative heat loss. 41.-42. (canceled)
 43. The method of claim 32,wherein the transferring the cooled one or more getters from the cooledat least one activation region to the structural region through theconnector, while maintaining the established vacuum within thegas-sealed apparatus comprises: bending the connector to alter therelative positioning of the cooled at least one activation region to thestructural region in relation to the connector.
 44. The method of claim32, wherein the transferring the cooled one or more getters from thecooled at least one activation region to the structural region throughthe connector, while maintaining the established vacuum within thegas-sealed apparatus comprises: transferring the cooled one or moregetters into a gas-sealed gap between an inner wall and an outer wall ofthe structural region. 45.-46. (canceled)
 47. The method of claim 32,further comprising: adding sealing material to a surface of theseparated connector adjacent to the structural region including thecooled one or more getters.
 48. The method of claim 32, furthercomprising: heating the structural region to a preset temperature for apredetermined time after establishing vacuum within the structuralregion and before heating the at least one activation region. 49.(canceled)
 50. The method of claim 32, further comprising: heating thestructural region to a preset temperature prior to transferring thecooled one or more getters; and maintaining the preset temperature whileseparating the connector.
 51. A method of establishing and maintaining avacuum within a storage device, comprising: assembling substantially allstructural components of a storage device, including an outer wall andan inner wall substantially defining a gas-sealed gap; attaching thestorage device to a gas-sealed apparatus, the gas-sealed apparatusincluding a getter activation region containing one or more getters, avacuum pump, and a connector operably connecting the storage device tothe gas-sealed apparatus; activating the vacuum pump to establish a gaspressure below atmospheric pressure within the gas-sealed gap of thestorage device; heating the storage device to a predeterminedtemperature for a predetermined length of time; heating the getteractivation region and the one or more getters to an activationtemperature for an activation time suitable to activate the one or moregetters within the getter activation region, while maintaining theestablished gas pressure below atmospheric pressure within thegas-sealed gap of the storage device; allowing the getter activationregion and the one or more getters to cool to a predeterminedtemperature; flexing the connector to move the storage device and thegetter activation region into a relative position wherein the getteractivation region is above the storage device and the connector issubstantially linear; allowing the one or more getters to fall along theconnector interior into the gas-sealed gap in the storage device, whilemaintaining the established gas pressure below atmospheric pressurewithin the gas-sealed gap of the storage device; separating theconnector at a location adjacent to the storage device while maintainingthe established gas pressure below atmospheric pressure within thegas-sealed gap of the storage device.
 52. (canceled)
 53. The method ofclaim 51, wherein the activating the vacuum pump to establish a gaspressure below atmospheric pressure within the gas-sealed gap of thestorage device comprises: establishing a gas pressure of less than orequal to 1×10⁻² torr. 54.-56. (canceled)
 57. The method of claim 51,wherein the heating the getter activation region and the one or moregetters to an activation temperature for an activation time suitable toactivate the one or more getters comprises: heating the getteractivation region with a heat source external to the getter activationregion.
 58. (canceled)
 59. The method of claim 51, wherein the flexingthe connector comprises: flexing a region of the connector adjacent tothe getter activation region.
 60. The method of claim 51, wherein theseparating the connector at a location adjacent to the storage devicewhile maintaining the established gas pressure below atmosphericpressure within the gas-sealed gap of the storage device comprises:physically crimping the connector; and breaking the connector at thelocation of the physical crimping.
 61. The method of claim 51, whereinthe separating the connector at a location adjacent to the storagedevice comprises: utilizing an ultrasonic welding device.
 62. The methodof claim 51, further comprising: heating the storage device to apredetermined temperature for a predetermined length of time afterestablishing the gas pressure below atmospheric pressure within thegas-sealed gap of the storage device.
 63. The method of claim 51,further comprising: monitoring the gas pressure within the gas-sealedgap of the storage device.
 64. The method of claim 51, furthercomprising: monitoring the gas pressure within the connector.
 65. Themethod of claim 51, further comprising: adding sealing material to asurface of the separated connector adjacent to the storage device.